Professional Documents
Culture Documents
(INORGANIC CHEMISTRY)
THEORY (3hrs/wk)
INORGANIC CHEMISTRY:
1. Introduction: (2 hours) Pharmacopoeia and monograph.
2. Quality control and test for purity: (4 hours) Sources of impurities in Pharmaceutical
substances.
Limit tests: Definition, importance, general procedure for limit test for chlorides, sulphates, iron,
arsenic, heavy metals, lead and modifications with suitable examples.
3. Radiopharmaceuticals and contrast media: ( 3 hours )Nuclear reactions, nomenclature, units
and measurement of radioactivity, clinical applications and dosage, hazards and precautions,handling
& storage, radio pharmaceutical preparations and standards of radioactive material iodine131(I131),
Cobalt -58(Co58). Radio opaque contrast medium-barium sulphate.
4. Study of pharmaceutically important compounds: Method of preparation, properties, assay (of
compounds with asterisk ), identification test, test for purity, official preparation, storage conditions
and uses of inorganic compounds listed in I.P belonging to the following categories. (Assay of
compounds marked* only)
a. Gastrointestinal agents and related compounds (10 hours)
(i) Acidifiers: Dilute hydrochloric acid, Ammonium chloride*
(ii) Antacids: Classification, Qualities of an ideal antacid, side effects, advantages of
combination therapy, acid neutralizing capacity, sodium bicarbonate*, Potassium citrate,
Aluminium hydroxide gel*, Magnesium hydroxide*, magnesium trisilicate, light and heavy
magnesium carbonate, Calcium carbonate, Dimethicone, Magaldrate, Bismuth carbonate.
(iii) Adsorbents and protectives: Light Kaolin, Activated charcoal, Bismuth subcarbonate, Titanium
dioxide.
(iv) Saline cathartics: Magnesium sulphate, Magnesium carbonate.
b. Topical Agents (9 hours)
(i) Protectives: Talc, Zinc Oxide, Calamine, Zinc Stearate, Silicon Polymers and Dimethicone.
(ii) Astringents: Alum, Zinc Sulphate and Zinc chloride*.
(iii) Anti-microbials: Hydrogen Peroxide*, Potassium Permanganate, Chlorinated Lime, Boric
Acid*, Silver Nitrate, Povidone-Iodine, Selenium Sulphide* and Zinc Undecenoate.
c. Dental products (3 hours)
i. Anti-caries Agents: Role of Fluorides as anti-caries agents, Sodium fluoride*.
ii. Dentifrices: Calcium carbonate, dibasic calcium phosphate, Zinc chloride.
d. Major intra and extra cellular electrolytes: ( 6 hours )
i. Physiological role of Chloride, Phosphate, Bicarbonate, Sodium, Potassium, Calcium and
Magnesium.
ii. Electrolytes used for replacement therapy: Sodium chloride, Potassium chloride, Calcium
chloride, Calcium gluconate*, Calcium lactate, Tribasic calcium phosphate.
iii. Physiological acid-base balance and its importance.
iv. Electrolytes used in the acid-base therapy: Sodium acetate, Potassium acetate, Sodium citrate,
Potassium citrate, Sodium lactate, Ammonium chloride. Electrolyte combination therapy,
Compound sodium chloride solution, Sodium chloride injection and Oral rehydration salt.
e. Gases: (4 hours) Oxygen*, Carbon dioxide, Nitrogen* and Nitrous Oxide*.
f. Essential and Trace ions: (8 hours) Definition, Physiological role of Iron, Copper, Zinc,
Chromium, Manganese, Molybdenum, Selenium, Sulphur and Iodine. Ferrous fumarate, Ferrous
gluconate, Ferrous sulphate*, Iron and Ammonium citrate, Zinc chloride and Potassium iodide.
Pharmaceutical Chemistry-I
Pharmaceutical Chemistry-I
PHARMACEUTICAL CHEMISTRY- I
PHARMACEUTICAL INORGANIC CHEMISTRY
Pharmacopoeia & Monograph
Pharmacopoeia is a book of directions and requirements for the preparation of medicine. The
word pharmacopoeia is derived from Greek word pharmakon which means a drug and poieo which
means to make. It is the legally recognised book of standards for the quality of the drug and their
preparation or included in it. It is published by an authority of a country which sets standards and
limits for drugs, raw materials and various pharmaceutical preparations.
These regulations and quality control parameters for drugs and dosage forms are presented
separately in general and specific articles (monographs) are published by an authority (government)
in the form of a book called as pharmacopoeia.
Pharmacopoeia published by the Indian government is called Indian pharmacopoeia (I.P).
Similarly British pharmacopoeia and United States pharmacopoeia are published by the respective
British & U.S government.
The government of India constitutes a committee called as Indian pharmacopoeia committee
(I.P.C) which prepares Indian pharmacopoeia and updates it regularly.
In pharmacopoeia each pharmaceutical or a drug is described under monograph.
The standards for chemical apparatus the techniques and processes are mentioned under
appendices.
Only the pharmaceutical which are commonly and currently used are included in
pharmacopoeia. The chemicals used for internal conceptions by human beings form the part of
pharmacopoeia.
The undesirable chemicals, poisons and commercial chemicals are excluded from the
pharmacopoeia.
HISTORY OF PHARMACOPOEIA
United state pharmacopoeia was published in 1820 and first B.P was published in 1864. The
first edition of I.P. was published in 1955 and its supplement was published in 1960.
Second edition of I.P. was published in 1966 and its supplement in 1975. The third edition of
I.P. was published in 1985. The fourth edition of I.P. was published in 1996.
5th edition of I.P. was published in 2007.
6th edition of I.P. was published in 2010 and its supplement in 2012.
7th edition of I.P. will be published in 2014.
Indian pharmacopoeia 1996 contains notices, preface acknowledgement introduction, general
notices, monograph (A to 0).
Volume II contains monograph (P to Z) infrared, reference spectrum, appendices, I.P. 2007
contains three volumes.
LAWS RELATED TO PHARMACOPOEIA
In Indian monographs given in Indian pharmacopoeia is subject to laws like drugs &
cosmetics act 1940. Dangerous drugs act 1930 and poisons act 1919.
MONOGRAPH
It is a complete description of a specific drug or dosage form. A drug or dosage form included
in a pharmacopoeia is termed as official and the sections dealing with official drugs and
pharmaceutical dosage forms are included in a pharmacopoeia. The monograph gives the complete
details like name of the compound chemical formula and molecular weight, physical characteristics,
dose test for purity. Identification test storage condition and assay.
Pharmaceutical Chemistry-I
Pharmaceutical Chemistry-I
For solutions;
Eg: Hydrogen peroxide solution is an aqueous of hydrogen peroxide which contains NLT 5%
W/V and not more the 7% w/v of hydrogen peroxide.
The compound if the composition is not known then the standard is roughly defined.
Eg: Dried aluminium hydroxide gel consist of hydrated aluminium oxide and small quantities
of aluminium carbonate and bicarbonate and standard is denoted as not less than 47% of aluminium
oxide.
8. IDENTIFICATION TEST
It involves specific chemical test like colour reaction test precipitation reaction and gas evolving test.
These tests are qualitative test.
Eg: Phenolic compounds react with ferric chloride to give violet colour.
9. pH
It is mentioned in monograph for solution and liquid dosage form preparation.
Eg: 4% AgNO3 as a pH between 5.4 to 6.4.
Test for purity/limits for impurity
It includes tests like acidity or alkalinity and specific impurity tests like limit test for chloride
sulphide heavy metal and arsenic.
Maximum amount of impurity of compounds and dosage forms are mentioned.
10. Assay
The percentage purity of the chemical or dosage form is mentioned in a monograph. It is a
quantitative test which involves titrimetric analysis and instrumental analysis.
11. Storage
It is used for preserving a chemical or dosage form.
In monograph the condition and nature of the containers are specified.
There are temperatures conditions like,
Cold (2-80C)
Cool (8-250C)
Warm (30-400C)
Room temperature
The type of containers for storage a chemical like well closed container, light resistance containers
and amber colour bottles are mentioned.
Eg:
1) Insulin injection is stored in cold place and should not be allowed to freeze.
2) Ferrous fumarate is stored in Amber coloured bottles.
QUALITY CONTROL AND TEST FOR PURITY
Quality control of various pharmaceutical drugs and dosage form should be in accordance with
official book (Pharmacopoeia).
The quality control and analytical control that is description solubility, standard, identification
test, test for purity and assay procedures should be according to pharmacopoeia monograph. It is
necessary to fix the standards and to have knowledge about the source of impurities and their effects
and possibility of their removal.
IMPURE COMPOUND
Compound is said to be impure if it is having foreign substances called as impure compound.
Chemical purity means free from foreign substances.
It is very costly to manufacture absolutely pure chemical substance.
Even standard compounds have minute quantities of impurities.
The substance employed in the preparation of a pharmaceutical must be pure and safe.
It is difficult to prepare pure chemical substance.
Impurities are incorporated during manufacturing purification or storage. The pharmacopoeia
describes various tests for purity of substances and mentions the limits and tolerance of certain
Pharmaceutical Chemistry-I
impurities like chloride, sulphate, Iron, heavy metals, lead and arsenic. These impurities should be
present in very small amount.
Properties of impure compound and its effects
1) Impurity is or toxic substances and produces various harmful reaction in human beings.
Eg: Arsenic and lead causes neurological problems
2) Nontoxic Impurities reduces the therapeutic activity of pure compound is reduced.
3) Impurities reduce or change the physico- chemical properties of substances.
4) Impurities react with pure substances and produce incompatible reactions.
5) Impurities cause changes in organoleptic properties of substances.
Eg:- Sodium salicylate is discoloured due to the phenolic impurities.
6) Impurities cause difficulty with the uses of the substance.
Eg: - potassium Iodate (KIO3) impurity in KI
Various sources of impurities are
1) Raw materials
2) Reagents used in manufacturing process
3) Inter mediate products in manufacturing process.
4) Defects in manufacturing process
5) Solvents
6) Chemical process used in manufacturing process
7) Action of solvents and reagents on the reacting vessels.
8) Atmospheric contamination
9) Faulty storage
10) Adulteration
1) Raw materials :Raw materials containing impurities will be passed during the manufacturing process to the
final products. Thus the final compound will be contaminated with those impurities.
Impurities such as arsenic lead heavy metals are present in the row materials and hence the
final compound will be contaminated will these impurities.
Eg: - Cu + 2H2SO4 CuSO4 + 2H2O+ SO2
Copper sulphate is prepared by the reaction between copper turnings with conc. H2SO4.
Copper turnings contain impurities like iron, arsenic. Hence the final compound CuSO4 will
be contaminated with these impurities.
Eg:- Zn + H2SO4 ZnSO4 + H2
ZnSO4 is prepared by the reaction between Zn and Dil. H2SO4 Zn metal contains impurities
like aluminium, copper, Mn, Mg, Ni, Arsenic and Fe. These impurities will be carried during
the preparation and the final product ZnSO4 is contaminated with these impurities.
2) Reagents used in manufacturing process:The reagents used in manufacturing process, if not removed completely by washing. It will be
present in the final product and act as impurities.
Eg: Cacl2 + Na2CO3 CaCO3 + 2 Nacl
(Soluble)
(ppt)
(soluble)
Precipitate of calcium carbonate is prepared by the interaction of solutions of cacl2 with
Na2CO3. The ppt of CaCo3 is washed to remove the excess of Na2CO3 and cacl2. If the ppt is
not properly washed it may persist as an impurity. The pharmacopoeia prescribes the limits o
tolerance of NaCl and chloride as impurities.
3) Intermediate products in the manufacturing process
6KOH + 3I2 5KI + KIO3 + 3H2O
KIO3 + 3C KI + 3CO
The intermediate substance produced during the manufacturing process will remain in the
final product and act as impurity.
Pharmaceutical Chemistry-I
Eg: Potassium Iodide is prepared by the reaction between KOH and Iodine. The resulting
solution is evaporated to dryness. The residues heated with charcoal KIO3 formed will be
converted to KI on treatment with charcoal. KIO3 is formed as an intermediate product and
not converted into KI. It will be present in an impurity in the final product. Hence
pharmacopeia prescribes the test for iodate.
4) Defects in Manufacturing process
The defect like incompleteness of reaction due to improper mixing and manufacturing
process like temperature, pressure or other reaction conditions will result in production of
impure compound.
Egs: 1. 2Zn + O2 2Zno 2. CaCO3+2HClCaCl2+H2O+CO2
Zno is produced by heating metallic Zinc in the current of air Zinc metal. If Zinc metal is not
heated properly it will not be converted to Zinc oxide. Hence the small amount of Zinc metal
will be present the final product as impurity. Hence I.P describes the test for Zinc metal.
5) Solvents
Water is a cheapest solvent and this used to prepare various dosage forms like
suspension, emulsion and other liquid dosage forms. Water may contain impurities like
chloride, sulphide, Bicarbonate calcium and magnesium. Hence the preparation of dosage
forms either distilled water or demineralised water should be used.
6) Chemical process
For synthesis of a drug many chemical reactions are involved like Nitration, Halogenation,
Oxidation, Reduction, Hydrolysis are involved. During the chemical process impurities will
be incorporated into the final product.
Eg: Potassium Iodide is obtained from sea weeds.
When Nitrogenous organic matter (sea weed) is burned with alkalis, Cyanide will be formed
and it will be present along with potassium Iodide.
Limit test for cyanide is described for KI in I.P
7) Action of solvents & Reagents on reacting vessel
Reagents and solvents will react with the container during preparation or storage.
Eg: 1) Strong acids leach out alkalis from Borosilicate glass.
2) Copper and Zinc vessels react with slightly acidic substance.
8) Atmospheric contamination
The atmosphere may contain Co2, So2, H2S or dust particles,. Depending on the area were the
preparation is carried out. These atmosphere impurities will affect the final product.
Eg: A solution of NaOH absorbs atmospheric Co2 to form Na2CO3
2 NaOH + CO2 Na2Co3+ H2O
Hence NaOH should not be exposed for a long duration during its manufacturing. I.P
prescribes NaOH should not contain more than 3% of Na2Co3.
9) Faulty storage
The improper storage of substances will change the physio-chemical properties and impurities
will be formed during the storage period.
Eg: Ferous sulphate, which exposed to moisture ferric sulphate, will be formed.
Hydrogen peroxide and silver nitrate are stored in black glass container or bottle.
KI and ferric ammonium surface liquefies on exposited to air.
10) Adulteration
For the purpose of increasing the bulk (volume) and to decrease the cost, adulterants are
added. Highly molecular weight, Substances or cheaper agent and sub stranded material are
added to the drug substances. Adulteration beyond permissible impurity is punishable under
food and drugs cosmetic act 1940.
Pharmaceutical Chemistry-I
LIMIT TEST
Limit test (Definition)
These are quantitative or semi- quantitative test designed to indentify and control small quantity of
impurities which are likely to be present in the substance.
Importance of limit test
Limit test are used for quality control of substances of raw materials.
It is used to identity impurities
It is used to determine the permissive limits of tolerance of impurities.
It is used to deduce toxic impurities like heavy metals, arsenic, lead which are likely to be
present in the substance.
It used to identify substances which are safe and pure for pharmaceutical preparation.
These tests involve a simple comparison of opalescence colour, turbidity with that of standard
mentioned in pharmacopoeia.
In these test concentration of impurity which expressed as ppm are percentage
Factors involved in limit test
1) Limit test is specific in nature.
2) Limit test should be sensitive in nature.
3) There should be control of personal errors.
Limit test of chlorides
Principles:
It is based on simple reaction between Ag No 3 and the soluble chlorides to obtained AgCl which is
insoluble in dilute nitric acid(HNo3). The AgCl produced in the presence of dil. HNO 3 makes the
solution turbid or opalescence is formed.
The extent of opalescence depends upon the amount of chloride present in the test substance. It is
compared with the std. Opalescence, produced by the addition AgNO3 to a std. solution of chloride
(Nacl).Same volume of dil. HNo3 is used in the both standard and test solutions. The opalescence
produced the test substance is less than the standard opalescence. The substance passes the limit test
for chloride. The opalescence produced in test is more than the standard, then the substance fails the
limit test for chloride.
Eg:
Standard
Nacl + AgNO3
AgCl +NaNo3
Test
Pharmaceutical Chemistry-I
Procedure
Take two Nesslers cylinder and label to as standard and test. According to I.P 1996
Sl.N
Standard
Test
Reason
o
1
Pipette out 1ml of 0.0824 percentage
Prepare a solution as The aqueous solution
solution of Nacl into the Nesslers
directed in individual
will leach out all
cylinder and add 9ml of distilled water monograph(Take 1g chloride ion present
and mix well
+ 10ml of distilled
in the sample. So
water)
that the cl ion can
react with AgNO3
and opalescence can
be compared
2
Add 10 ml of dil. HNO3
Add 10 ml of dil.
HNO3 prevents the
HNO3
precipitation of other
radicles like
sulphate, phosphate
etc and also prevents
dissociation of AgCl.
3
Dilute to 50 ml with distilled water
Dilute 50 ml with
The limit test is a
(Free from ions)
distilled water
comparison and
hence equal volumes
can be compared
easily.
+
4
Add 1ml of 0.1 molar AgNO3 solution
Add 1 ml of 0.1
Ag ions reaction
stir well and allowed to stand for five
molar AgNO3 . Stir
with Cl- ions to form
minutes
well and allowed to opalescence of AgCl.
stand for five
(Ag++ Cl- AgCl)
minutes
Opalescence in the sample adds the standard solutions are compared by keeping the Nesselers
cylinder against black background and viewing transversely. The opalescence produced in the test
solution is less than standard solution when the substance passes the limit test for chloride. The
opalescence produce the test solution more than the standard solution then the substance failed the
limit test for chloride.
LIMIT TEST FOR SULPHATE
Principle
It is based on the reaction between Barium chloride and soluble sulphate in the presence of dilute
Hcl. It results in the formation of turbidity due to BaSO 4. Then turbidity produced by the given
amount of test substance is compared with the standard turbidity. Standard turbidity is obtained from
a known amount of sulphate and same volume of dilute Hcl added to a solution of Bacl2.
Bacl2 is used in the form of a BaSo4 reagent which contain Bacl2 sulphate free Alcohol and the
solution of K2SO4. K2SO4 added increases the sensitivity of the test. The ionic concentration in the
reagent is adjusted. Such that the solubility product of BaSo 4 gets exceeded. The very small amount
of K2SO4 present in the reagent act as a seeding agent for the preparation of BaSo4. Alcohol helps to
prevent super saturation and thus produces a more uniform turbidity. The substance passes the limit
test for sulphate. If the turbidity produced in the test solution is less than that of standard. The
substance fails the limit test if the turbidity produced is more than the standard.
Standard
K2SO4 + BaCl2 HCl/ BaSO4 +2KCl
Pharmaceutical Chemistry-I
Test
Procedure
Take two Nesslers cylinder and labelled it as standard and test
Standard
Test
Pipette out 1ml of 25%. W/v Pipette out 1ml of 25%. W/v
solution of Bacl2 into a solution of Bacl2 into a
nessler s cylinder.
nesslers cylinder
Add 1.5 ml of ethanolic Add 1.5 ml of ethanolic
sulphate standard solution
sulphate standard solution
Add 15 ml of standard
sulphate solution
(0.1089%.K2SO4)
Add .15ml of 5 molar acetic
acid
Add 15 ml of solution
prepared of as directed in
individual monograph
Add .15 ml of 5 molar acetic
acid
Reason
Bacl2 act as precipitating
agent. Ba2+reacts with SO4
to form turbidity of BaSO4
Ethanolic solution of K2so4
increases the sensitivity of
test and alcohol prevents
super saturation of baso4
It gives sulphate ion present
in the sample or standard in
the solution form
Acetic
acid
prevents
precipitation of phosphate,
cl-,borate, oxalate
Equal volumes can easily
compared.
Observation:
The turbidity produced in test is compared with standards by viewing against black back ground
transversely. Sample passes the limit test, if the turbidity produced with the test is less than the
standard turbidity.
LIMIT TEST FOR IRON
Principle
It is based on the reaction of Iron in ammonical solution in presents of citric acid. Here Iron react
with Thioglycolic acid to give a pale pink to deep reddish purple colour. The colour is formed due to
the presence of ferrous compound. Citric acid does not allow the precipitation of Iron by ammonia
By forming a complex. Thioglycolic acid reduces ferric Iron (Fe 3+) to ferrous iron (Fe22+). The
ferrous state gives the purple colour does not gets oxidised back to ferric state in absence of air or
oxidising agent. Thioglycolic acid is a sulphur analog of glycolic acid, it is prepared by the action of
potassium hydrogen sulphide (KSH) on mono chloro acetic acid. The ferrous thioglycolate complex
gives purple colour in alkaline condition by the addition of NH 3 solution. The purple colour produced
from a specified amount of substance from the test is compared by viewing vertically with the
standard substance. (Ferric ammonium sulphate)
The purple colour produced in test is less than the standard Then substance passes the limit test for
iron. Purple colour produced in test more than the standard. Then the substance fails the limit test for
iron.
Pharmaceutical Chemistry-I
10
Reason
Aqueous solution will leach
out all the iron present in the
sample or test
Reaction
Preparation of thioglycolic acid
CH2ClCOOH + KSH ------CH2 (SH) COOH + KCl
Observation
The intensity of purple colour produced is compared with the standard. The intensity of purple colour
produced in test is less than the standard. The substance passes the limit of Iron. If intensity produced
in the test more than the standard, then the substance fails the limit test of iron
LIMIT TEST FOR ARSENIC (As)
Principle
Arsenic produces cumulative toxicity and hence the presence of arsenic in a drug is not desirable.
Indian pharmacopoeia prescribes the limit for the presence of As as an impurity in various drugs.
Pharmaceutical Chemistry-I
11
Eg: NaCl should contain not more than 1 ppm of Arsenic. Limit test for arsenic is performed by
using Gutzeit apparatus.. Arsenic present in standard or sample is dissolved in an acid (Hcl). In
acedic condition the trivalent form of arsenic is converted to arsenious acid and pentavalent form of
arsenic to arsenic acid depending upon the valence state.
H3AsO3+3H2---AsH3+3H2
The penta valent form of arsenic acid is reduced to trivalent form arsenious acid. The help of
reducing agent like sncl2 and KI
Arsenic acid reduced to form arsenious acid
The trivalent form of arsenic acid react with nascent hydrogen, which produced by the reaction
between granulated Zinc and Hcl and results in the formation of arsine gas or arsenious gas or
arsenious hydride.
Arsine gas reacts with dry mercury chloride paper to form yellow strain.
The hydrogen sulphide is formed along with arsine gas and interfere in the reaction between arsine
gas and mercury chloride. The hydrogen sulphide gas is trapped or blocked by reaction with lead
acetate cotton an gets converted to lead sulphide (Pbs)
The intensity of yellow strain produced in standard (Arsenic trioxide) and test is compared. The
intensity of yellow strain produced in test solution is less than the standard. The substance passes the
limit test for arsenic and otherwise it fails
Pharmaceutical Chemistry-I
12
GUTZEIT APPARATUS
Construction
It is a wide mouth glass bottle of 100ml capacity. So its diameter of the mouth is about 2.5 cm. Glass
bottle is fitted with a rubber bung, through which passes a glass tube. Glass tube is 20cm long, having
external diameter of about 8mm and internal diameter of about 6.5mm. The glass tube is constricted
at the bottom extremity to about 1mm diameter.
It has the hole in the side tube near the constricted area. So the upper part of the glass tube fitted with
two upper part of the glass tube fitted with two rubber bungs. The rubber bung as a hole centrally
with diameter of 6.5 mm to hold the glass tube (25mmX25mm). Two rubber bungs are kept in close
contact by a spring clip. The two rubber bungs hold the mercuric chloride paper.
Pharmaceutical Chemistry-I
13
Procedure
All the reagents used must be free from As impurity.
The limit test for Arsenic is performed by using Gutzeit apparatus.
Separate apparatus are used for standard and test solution and both are performed
simultaneously. Prepare the test solution as directed in individual monograph.
Take 1g of KI (5ml KI solution) 5 ml of Sncl 2 acid solution and 10g of granulated Zinc
ZnAsT) in the glass bottle. The glass tube with lead acetate cotton and Hgcl 2 paper is quickly
fixed.
The apparatus is kept at 40oC in the water bath for 40 minutes.
Yellow stain is produced on the Hgcl2 paper. Which compared with the standard comparison
of yellow stain is done immediately at the completion of test and standard reaction.
Observation
The yellow stain produced in test less than the standard. The test substance passes the limit
test. The test is more than the standard if The substance fails the test.
LIMIT TEST FOR HEAVY METALS
Principle
Heavy metals are toxic substances like cobalt, tin, manganese, bismuth, lead, antimony may be
present in the pharmacopoeia substance. The principle involves the reaction between heavy metals
and H2S or Na2S resulting in the formation of metal sulphides which gives brown colour. Comparing
the intensity of brown colour produced in test and standard solution (standard lead solution). The
substance are analysed for heavy metals.
Method: 1 (For colourless substance)
Take two nesslers cylinder and label standard and test.
Fe2S+Hcl H2S + Fecl3
M + H2S Ms + H2
Heavy Metal
Metal Sulphide (Brown Colour)
Procedure
Method 1 (For colourless substance)
Take two nessler;s cylinder and label to as standard and test.
Standard
Test
Preparation 1ml of lead standard solution Take 25ml of test solution, or specified
(1% Lead nitrate)
quantity of substance mentioned individual
monograph
Adjust the pH with dilute ammonia solution Adjust the pH with dil ammonia solution or
of dilute acetic acid solution and pH dil. CH3COOH solution and pH maintained
maintained between 3 and 4
between 3 and 4
Dilute 10ml of Freshly prepared H2S solution Add 10 ml of freshly prepared H2S solution
and mix well
and mix well
Dilute 50ml with distilled water and allowed Dilute 50 ml with distilled water and
to stands for 5 minutes
allowed to stand for 5 minute
Observe the intensity of brown colour over white surface. The intensity of brown colour
produced in test solution is less than the standard. The substance passes the limit test for
heavy metal
Pharmaceutical Chemistry-I
14
Pharmaceutical Chemistry-I
15
Procedure
It is performed by extraction with separating funnel. To transfer the standard and test solution into
two separating funnel. Add 6ml of ammonium citrate solution and 2ml of hydroxyl amine hydro
chloride solution and two drops of phenol red. Make it alkaline by adding ammonia solution cool and
add 2ml of KCN soln immediately extract the solution with several quantities of 5ml of dithizone
extraction solution. Until retains a green colour. Shake the combined dithizone solution for 30s with
30 ml of 1% HNO3 solution and discard the chloroform layer. Mix the acidic solution with 5 ml of
dithizone std extraction solution and shake for 30s.
The violet colour of the chloroform extracts is not more intense than obtained by treating in the same
manner. A solution lead standard (1ppm lead nitrate)
Pharmaceutical Chemistry-I
16
If this lt test are done in normal way. It will be difficult to make any observation since the compound
itself is highly coloured. The colour of Mno2 is eliminated by reduction with alcohol. This is called as
pre treatment.
Sample is dissolved water and heated on water bath. Alcohol is added . Then the solution is filtered to
remove the precipitate of Mno2. The filtrate is colourless and can be used to perform lt test for
chloride and sulphate
Procedure
Take 1.2g KMnO4 and dissolving 50ml of distilled water. Heat on water bath and add 6ml of
ethanol. Cool and dilute to 60ml with distilled water and filtered. The filtrate is colourless. For limit
test chloride take 40ml of the above solution and perform normal lt test for chloride.
For limit test for sulphate, take 10 ml of the above solution and perform normal limit test for
sulphate.
(5)
(10)
(10)
(10)
(5)
(5)
3. Limit test
1. Define limit test & give its importance.
(5)
2. Explain the factors involved in the limit test.
(5)
3. Explain the role of stannated HCl, potassium iodide & mercuric chloride in the limit test for
arsenic.
(5)
4. Give reason for the use of lead acetate, cotton wool in the limit test for arsenic. (5)
5. Give the reason for the use of citric acid & ammonia in the limit test for iron. (5)
6. Give the composition & use of barium sulphate reagent in the limit test for
sulphates.
(5)
7. Write the principle involved in the limit test for chlorides.
(5)
8. Write the principle involved in the limit test for sulphates.
(5)
9. Explain the limit test for iron.
(5)
10. Explain the principle involved in the limit test for arsenic.
(5)
Pharmaceutical Chemistry-I
17
Pharmaceutical Chemistry-I
18
Radioactive material kept in lead chamber and the radiations are passed through oppositely charged
plate. The radiation deflected by charged plates. The radiation deflecting or bending towards the
positively charged plate is rays or particle (negatively charged). The rays do not bend either to
positive or negative charged plated. But passes through a straight line uncharged is called rays or
particles.
Properties of radioactive radiation or radioactive decay particle
rays
It is denoted by 42 or He24
rays have 2 positive charge and number of 4.
They have very high velocity equal to about 1/10th of light.
The penetrating powder through the matter is very low.
They are stopped by a sheet of paper.
They have the capacity to get ionised in molecule of gas through which pass and module ion
pairs.
Eg;
Pharmaceutical Chemistry-I
19
Units of radioactivity:Curie(C) This is equal to 1g of radium which undergoes 3.7x 10 10 disintegration per second.
milli curie(mC) is 10-3 or 1g of radiation undergoes 3.7 x 10-7 disintegration per second.
Micro curie it is 10-6 curie Or When 1g of radium undergoes 3.7 x 10-4 disintegration per second.
Becquerel(Bq): It is one disintegration per second.
Roentgen(R): It is the unit of radiation exposed
1R=2.58 x 10-4 coulomb/Kg
RAD: It is the unit of absorbed dose.
1RAD= 10-2 J/Kg
Measurement and detection of radioactivity:When radioactive substance decays, it emits a particle or EMR or both depending upon the mode of
decay of the nucleus. They are measured or detected by using radioactivity measuring equipments or
detectors for detecting a particular type of radiation.
The property of radiation are utilised in their detection and measurement. Eg ; the scintillation effect
is measured in scintillation counter, the ionising effect is measured in ionisation chambers,
proportional counters and GM counter and the photographic effect in autoradiography.
Radioactive detectors are classified based upon:
I.
Collection of ions
II.
Collection of photons.
Radioactive detectors utilising ion collection:
1. Gas filled detectors
a. Cloud or bubble chamber detector
b. Ionisation chamber detector
Pharmaceutical Chemistry-I
20
Pharmaceutical Chemistry-I
21
Geiger-Muller counter
Spinthariscope
Pharmaceutical Chemistry-I
22
Pharmaceutical Chemistry-I
23
Applications of radiopharmaceuticals
1) There are number of preparation containing radioisotopes which are used internally for
therapeutic and diagnostic purposes. These radioisotopes are called as radio pharmaceuticals.
2) Radio pharmaceuticals emitting or radiations are used for diagnosis and therapeutics
3) Radiopharmaceuticals are widely used in four major areas.
1) Radiopharmaceutical in therapeutics
2) Radiopharmaceutical in diagnosis
3) Radiopharmaceutical for research purpose
4) Radiopharmaceutical for sterilization purposes
Radiopharmaceutical in therapeutics
Radioisotopes of sufficient energy are used for various therapeutics purposes.
Radioisotopes cause destruction of tissues.
Radio isotopes are employed for various cancer treatments.
Gold 148 is used to the treatment of various neoplastic diseases like liver cancer.
Emitter I131, I135 are used for the treatment of hyperthyroidism and metastatic thyroid cancer.
Fluorine F18 is used for the treatment of brain tumour.
P32 used for cerebral tumour and chronic granulocytic leukaemia.
Tantalum 201 used for the treatment of cancer.
Radio isotopes for diagnosis: Radioisotopes are tagged into a molecule and directed into particular tissues with a high
degree of specificity.
Many materials are opaque visible light and are transparent to x-rays and rays.
Radioisotopes are used to trace particular disease organ.
I131, I135 in the form di iodo florescence map brain tumour.
Co57 diagnosis of pernicious anaemia.
Fe59 used for diagnosis of iron metabolism and RBC formation.
Iodised serum albumin used for the diagnosis of blood volume or cardiac out put.
Radio pharmaceutical for sterilization
1) Thermo labile drug like penicillin is sterilized by radioisotopes all microorganism and their
spores are killed within seconds and drugs become sterile. rays from radioisotopes used for
sterilization.
2) For sterilization of surgical equipments are sterilized by radiation.
Dosage of radioactivity:The radioisotopes used for internal administration and dosage to be given are called radiation
dosimetry. The dose has to be properly calculated in reference to both animate and inanimate objects.
This does is described by exposure dose and absorbed dose.
Exposure dose of radioactivity refers to the quantity potentially of harmful radiation in air
surrounding a particular area. Exposure dose is measured dose rate at a particular distance from
radiation source. The unit is roentgen/hr/m (rhm).
The absorbed dose of radiation is a specific unit employed in denoting the amount of radiation
absorbed by body unit is RAD.
The absorbed dose used in describing potential damage for biological tissues due to different types of
radiation. It is denoted by the relative biological effectiveness (RBE).
Pharmaceutical Chemistry-I
24
The dose(rad) multiplied by appropriate RBE gives a more biological useful dosage is obtained
called rem.(roentgen equivalent mean)
Hazards of Radioactivity:
Radiations have very dangerous effect on biological tissue depending upon the ability of radiations to
penetrate the tissues, energy of radiation, surface area exposed, type of tissue and the dose of
radiation. The radiation ionisation promotes a number of irreversible changes in living cells.
These chemical changes alter the local pH or serve to initiate free radical chain reactions and
forming peroxides and other toxic compounds. These and other events can create a hostile
environment for tissue cell, leading to necrosis and ultimately, complete destruction of the tissue or
organ. The free radicals formed from water can also abstract radicals from other molecules, resulting
in the production of a variety of potentially toxic species which can alter the DNA in cells and causes
cross linking between certain amino acids and proteins.
The constant multiplying tissues like bone marrow, Mucosa of the gut, foetus and gonads are most
affected by radiations. The side effects of radiations include nausea, vomiting and alopecia. These
effects may lead to change in protein sequence of DNA and subsequent generation also produces
similar effects.
Nuclear reaction:There are two types of nuclear reaction namely nuclear fission and nuclear fusion. A nuclear reaction
which proceeds with change in composition of nucleus. So as to produce an atom of new element.
This conversion of one element to another by a nuclear change is called Trans mutation.
Nuclear fission:Highly charged alpha particles are accelerated by high kinetic energy by means of cyclotron. This
charged particle enters into nucleus and produces an unstable compound nucleus. This compound
nucleus is broken into two or more fragments and the process os known as nuclear fission. Thus
nuclear fission is a splitting of heavy nuclear into small fragments approximately equal mass. The
fission products are radioactive themselves. They are rich in neutrons and decay by emitting beta
particle or neutrons and emits radiation and ultimately change in to a stable elements. The release of
fission energy can be uncontrolled manner and controlled manner.
Eg: nuclear reaction
Nuclear fusion:It is a combination of fusion of two small nuclear into a large nucleus initially there is a formation of
unstable nucleus which later forms a stable larger nucleus along with the emission of radioactive
rays. The energy required to induce the fusion reaction is applied in the form of heat and causes to
increase in thermal energy of particle at high temperature. The fusion reaction is thermonuclear
fusion.
Different between nuclear fission and fusion reaction
Nuclear fission
Nuclear fusion
A bigger nucleus splits into smaller nucleus
small nucleus fussed together to form larger
nucleus
No high temperature is required to carry out Extreme high temperature is required
nuclear fission reaction
Chain reaction occurs
No chain reaction occurs
It is controlled energy and can be used for Cannot controlled and energy released cannot
peaceful purposes
be used properly.
Pharmaceutical Chemistry-I
25
Nuclear waste is left behind after the reaction No nuclear waste is formed the reaction is
is completed
completed
Radioisotopes half life
The time required to disintegrate half of its active original isotope according to the law of
radioactive disintegration is called Radioisotopes half life
According to law of radioactive disintegration
N = Noe-t
At half life, when t = t1/2
N = Noe- t1/2
t1/2 = 0.693/
No is active isotope present at time t.
N is original active isotopes
is the rate of decay
Nomenclature of radioactivity
Symbol of element is given
Mass number of isotope is mentioned at the top.
The atomic number at the bottom on left side of symbol.
It is not necessary to mentioned the atomic number always and it is same for all isotopes of an
element alternatively name of the element followed by mass number of the isotope on the
right side with hyphen an in between.
Radioactive pharmaceutical preparation
Sodium iodide NaI(I131)
Standard : Content of iodine should be between 90 & 100 % of the stated on the label at the time
and hr of preparation. The specific gravity is not less than 5 mcg of iodine.
Preparation
By bombarding or by irradiating tellurium with neutrons radioactive isotopes, I 131 is obtained
then converted to salt form of sodium iodide.
Property
It is a clear colourless odourless solution
Usually given in oral administration
The preparation is stabilized by adding reducing substation like sodium thiosulphate.
It has half life of 8.06 days.
Emits both beta particle and gamma rays.
Identification test
Gama rays spectrum is compared with standard spectrum of I 131 which has a proton of energy of .
36meV. The aqueous solution has pH 7.10.
Radio nucleus purity
Gama rays of I is measured by suitable detector. The spectrum obtained on the preparation is
compared with standard radioisotopes. These are a significant difference between two spectrums. The
test is carried out to deduce the other type of radioisotope impurity.
Radio chemical purity
This test is carried out to ensure the preparation contains only iodide. There should not be any
iodate. This purity is confirmed by paper chromatography.
Uses:-
Pharmaceutical Chemistry-I
26
Pharmaceutical Chemistry-I
27
Pharmaceutical Chemistry-I
28
29
Pharmaceutical Chemistry-I
30
Uses
Gastric acidifier
Treatment of achlorrhydria
Used as pharmaceutical aid.
It is used as gastric acidifier by administering 5ml of dilute Hcl to 200ml of water which gives
about 15 milli equivalent of Hcl.
Storage
It is stored in well closed container.
AMONIUM CHLORIDE
(NH4cl)
Standard
It contains not less than 99% and not more than 101% of NH4Cl.
Preparation
1) Bye neutralising Hcl with NH3 and evaporating to dryness NH4Cl is obtained.
NH3 + Hcl NH4Cl
2) By heating Ammonium sulphate with Nacl, NH3 and Hcl is obtained which is condensed to
form NH4Cl.
2Nacl + (NH4)2 SO4 2NH3 + 2Hcl + Na2SO4
NH3 +Hcl -- > NH4Cl
Properties
White crystalline powder having a cool saline taste and hygroscopic in nature.
Soluble in water and glycerine and readily soluble in boiling water and sparingly soluble in
Alcohol
On hydrolysis Hcl is formed.
NH4Cl+H2O NH4OH + Hcl (Gastric acidifier)
Identification test
The aq. Solution gives the characteristic test for NH3 and Cl
Test for purity
It is tested for As, Fe, S, Pb, thiocyanate sulphated Ash, pH and loss on drying.
Freshly prepared aq soln is neutral to litmus and becomes acidic by hydrolysis.
NH4Cl + 2H2O---------NH4OH+H3O+ClPH
A 5% solution should have a pH between 4.5 to 6.
Test for thiocynate
It is tested by adding Hcl and ferric chloride solution no red colour should be obtained.
Sulphated ash: no more than 0.1%.
LOD; NMT 0.5%
ASSAY
Formal Titration
Weigh accurately about 0.1g of NH4cl and dissolved in a mixture of 20ml of water and 5ml of
formaldehyde solution. After 5 minutes titrate the contents of conical flask against 0.1 N NaOH using
phenolphthalein as indicator. The end point is appearance of pink colour. Each ml of 0.1N NaOH is
equivalent to () 0.005349g of NHJ4cl
Principle
NH4cl + H2O NH4OH + Hcl
4NH4OH + 6HCHO C6H12N4 + 10H2o
Pharmaceutical Chemistry-I
31
32
Pharmaceutical Chemistry-I
33
Dissolve NaHCO3 in 10ml of water and add 5 ml of potassium carbonate solution and add freshly
prepared potassium antimonite solution. A dense white precipitate is obtained.
Test fo carbonate
NaHCO3 is heated to liberate CO2, to the solution lime water is passed which produces milky white
precipitate.
Test for purity
NaHCO3 is tested for alkalinity of al, Cu, As, Fe, heavy metals, cl, so4, ammonium compounds and
insoluble matter.
Clarity and colour of solution
A 5% W/v of solution of NaHCO3 have pH not more than 8.6
Loss on drying
It is determined on 4 g of NaHCO3 by drying for four hours moisture should not be more than .25%
Test for Ammonium compounds
1g of NaHCO3 is formed with 10ml of NaOH solution. No ammonia fumes should be evolved.
Assay of NaHCO3
Acid base titration or neutralisation titration
NaHCO3 +Hcl Nacl + H2O + Co2
Weigh accurately about 1.5 of NaHCO3 and dissolving 50 ml of Co2 free freshly boiled and cooled
water. Add one or two drops of methyl orange indicator. Titrate the contents of flask against one
normal Hcl. The end point is appearance of pink colour. Standardise the one normal Hcl using
Na2CO3 solution.
Uses
1. It is used as antacid.
2. I.V (Intra venous) infusion of NaHCO3 is used as electrolyte replenisher
3. It is Used as electrolyte replenisher
4. It is used for treatment of systemic acidosis.
5. Used as wax softener in ear drops.
6. It is used in eye lotion, for washing of eye.
Storage; Stored in a well closed container protected from moisture.
Calcium carbonate
Chemical formula: CaCO3
Synonyms: Precipitated chalk
Standard
Contain not less than 98% and not more than 100.5% of CaCo 3 calculated with reference to dried
substance.
Preparation
Boiling solution of Na2CO3 is added to a boiling solution of Cacl2 and precipitate of caco3 is
obtained. The precipitate is washed and dried.
Na2CO3 + Cacl2 2Nacl + CaCO3
Co2 gases passed through lime water the white precipitate of CaCO3 is obtained.
Ca (OH)2 + Co2 CaCO3 + H2O
Properties
White colourless, odourless, amorphous powder.
Very slightly soluble in water.
Solubility of CaCO3 is increased in the presence of dilute acids.
CaCO3 reacts with dilute acids like Hcl, with liberation of Co2
CaCO3 +Hcl CaCl2 + H2O + CO2
Pharmaceutical Chemistry-I
34
When excess of CaCo3 of Co2 gas is passed into a solution of caco3. Ca(HCO3)2 is obtained
CaCo3 + Co2 + H2o Ca(HCo3)2
Antacid action;
Fast acting antacid: The gastric acid is consumed by soluble CaCO3. Ca can either be absorbed or
precipitated as insoluble form and produces constipation effect.
Identification test
To aqueous solution of CaCo3 , add dilute HCl. cO2 gas is liberated then add 5 ml of Barium
hydroxide solution white precipitate of is obtained.
Test for calcium
Take 1g of CaCo3 dissolving diluted Hcl and add 5 ml of ammonium oxalate solution a white ppt is
obtained which is sparingly soluble in dil HCl.
Test for purity
It is tested for acidity and alkalinity, Barium, Arsenic, Mg, Alkali earth metals, heavy metals,
aluminium, Iron, Phosphate, sulphate soluble alkali and loss on drying.
Test for Barium
2g of CaCo3,add 10ml of acetic acid solution and boil the solution, cool and add 10ml of calcium
sulphate solution. The solution should remain clear.
Test for Ca, Mg, and Alkali earth metals
To 1g of CaCo3 add 10ml diluted Hcl, neutralise the solution by adding ammonia solution. The
solution is heated then add a solution of ammonium oxalate, to this add 1.5ml diluted H 2So4, and
evaporate the solution on a water bath. The residue obtained should not be more than 10mg.
Side effects:
Gastric haemorrhage, hypertension, dehydration, Burnett syndrome.
Uses
1) It is used as fast acting antacid
It act as an antacid and the gastric Hcl consumes the soluble CaCo3, this process is continued
until all the acid is completely neutralised.
CaCO3 +Hcl CaCl2 + H2O + CO2
2) Used as dentifrices becauses of mild abrasive property.
Storage
Stored in a well-closed container protected from moisture
Magnesium carbonate
Chemical formula - MgCO3
It occurs in two forms,
1) Heavy magnesium carbonate
2) Light magnesium carbonate
Both magnesium carbonates differ in their hydration and density.
1) 3 MgCO3
Mg(OH)2
5H2O
(Heavy)
2) 3 MgCO3
Mg(OH)2
3H2O
(Light)
Degree of hydration depends upon water molecules are present. 15g of heavy magnesium carbonate
occupies the volume of 30ml of water.
15g of light magnesium carbonate occupies a volume of 125ml of water.
Pharmaceutical Chemistry-I
35
Identification test
Heavy Magnesium carbonate is dissolved in dilute acids like acetic acid and gives a characteristic test
for Mg and carbonate
Test for Magnesium and Carbonate
To 1g of heavy mgCo3 add 10 ml of diluted Hcl neutralise the solution by adding NH 3 and solution is
heated. Add a solution of NH 3 oxalate add 1.5ml H2SO4 evaporate the solution in water bath reduce
obtain not more than 10mg
Test for purity
Heavy magnesium carbonate is tested for Arsenic, Calcium, Iron, Copper, Lead, Chloride sulphate,
soluble matter and residue on ignition.
a) Test for calcium
To 5 ml of ethanolic calcium standard solution. Add 1ml of ammonium oxalate. After 1 minute
add mixture of 1ml of 2m acetic acid. Take 1.5ml of the above solution and dilute to 150ml with
distilled water and shake well. No precipitate should be obtained.
b) Test for soluble matter
1g of MgCo 3, add 50ml of distilled water. Boil the solution for 5 minute. Filter the solution
and collect the residue obtained and dry at 105oC for three fours. The residue should not be more than
10mg
Test for Cu:
Dissolve in dil.HCl and make it alkaline with dil.NH3 soution. No blue colour should be obtained.
c) Residue on ignition
Ignite 0.5g of heavy magnesium carbonate to a constant weight at 900 oC. The residue obtained
should not be less than 42% and not more than 45% .
Uses
Pharmaceutical Chemistry-I
36
1) It is a weak antacid
2) It is used as laxatives
3) It is used as adsorbent in preventing the formation of eutectic mixture
Storage
Stored in a well closed container
LIGHT MAGNESIUM CARBONATE
C.F MgCo3
Mg(OH)2
3H2O
Std ;
It contains not less than 40% and not more than 45% of Mgo Calculated with reference to dried
substance.
Preparation
It is prepared in the same manner as heavy MgCo 3. 125 parts of MgSo4 and 150 parts of Na2Co3 are
dissolved separately in thousand parts of cold water. It is mixed and boiled for 5mts to obtain light
MgCo3.
MgSo4 + Na2Co3 MgCo3 + Na2So4
Properties
Very light white powder, odourless, and tasteless powder.
Practically insoluble in water and alcohol . Soluble in dilute acids with generation of
effervescence.
When heated to redness, it forms Co2 and MgO
Identification test, Test for purity same as Heavy.MgCo3
Uses
It is used as antacids
It is used as laxatives
Storage
Stored in a well closed container protected from moisture
Magnesium hydroxide
Chemical formula: Mg(OH)2
Synonyms: Milk of magnesia, Cream of magnesia
Standard
It Contains not less than 95% and not more than 100.5% of Mg (OH)2 Calculated with reference to
dried substance.
Preparation
1) Is prepared b reacting MgSO4 with NaOH precipitate of Mg (OH)2 is obtained the preparation
is filtered and washed with water until free from sulphates.
MgSO4 + 2NaOH Mg(OH)2 + Na2So4
2) Hydrolysis of MgO by using water, (Mg(OH)2) is obtained
Properties
White fine amorphous powder insoluble in water and slightly alkaline.
It dissolves in mineral acids like H2SO4
Mg(OH)2 + H2SO4 MgSO4 + 2H2O
It absorbs CO2 from moisture
Identification test
Pharmaceutical Chemistry-I
37
Mg(OH)2 dissolved in dilute H2So4 gives a characteristic test for Mg and hydroxide.
Test for Mg
To 1g of sample neutralise the solution by adding NH 3 solution heated. Add NH3 oxalate and 1.5ml o
dilution. H2SO4 evaporate the solution a water bath. Residue obtain not more than l
Test for purity
It is rested for clarity and colour of solution Arsenic, heavy metals, Chloride, Sulphide, Calcium,
Iron, Soluble substances. Substances insoluble in acetic acid and loss on ignition.
Antacid action
It gets dissociated in stomach to Mg ions and hydroxide ions. The anion will be consumed by acid
and gets converted to water.
Assay
Acid base back titration method
To an accurately weighed amount of Mg(OH) 2 taken in a flask to this add 25ml of one normal
H2SO4 . Excess amount of acid back titrated with 1 normal NaOH using methyl red as indicator. The
end point is appearance of red colour.
Mg(OH)2 + H2So4 MgSo4 + 2H2O
2H2SO4 + 2NaOH Na2SO4 +2H2O
Uses
It is used as antacid.
Large dose of Mg(OH)2 is used as laxative.
It is used the preparation of milk of magnesia it contains not less than 7% and not more than
8.5% of Mg(OH)2
Storage
Stored in a well closed container, protected from moisture.
Magnesium trisilicate
C.F: 2Mgo 3SiO2 XH2O
Synonyms: Hydrated magnesium silicate Epsons salt (Epsom salt : Magnesium sulphate)
Standard
Magnesium tri silicate contains varying with varying amounts of water of crystallisation contains not
less than 29% and not more than 32% of MgO and not less than 65% and not more than 68.5% of
tisilic acid
Preparation
Magnesium trisilicate is prepared by reacting equimolar solutions of sodium silicate and mg sulphate.
The solution is filtered wash and dried.
Epson salt
MgSO4 + 2 NaSiO2 MgO 3SiO2 + Na2SO4
Mg Trisilicate
Properties
It is a fine white powder, free from gritty particles (Heavy particles).
it is odourless, hygroscopic, practically insoluble in water and ethanol.
When treated with Hcl, it gets decomposed to Mgcl2 and trisilicacid .
Pharmaceutical Chemistry-I
38
Antacid action:
The above reaction also occurs inside the stomach, when magnesium trisilicate reacts with Hcl, the
excess gastric acid is neutralised and a gelatinous mass is formed on reacting with gastric contents.
The gelatinous mass forms a protective coating on GIT and adsorbent effect on the gastric mucosa.
Colloidal SiO2 protects from further acid and pepsin.
Identification test
Mg trisilicate dilute Hcl gives the characteristic test for mg and silicon dioxide.
Test for Mg:
To 1 g of Ca Co3 add 10ml of dilute. Hcl neutralise the solution by adding NH3 Solution heated. Add
NH3 oxalate and 1.5 ml of H2SO4 evaporate the solution in a water bath, residue obtain not more than
10mg.
Test for purity
It is tested for arsenic , Iron, Heavy metals Cl, S, acid absorption or acid neutralising capacity.
Test for free alkali and soluble salts and loss on ignition
Test for free alkali
10mg of MgO3SiO3 is boiled with 150ml of water for 15mnts. Is cooled and filtered. The filtrate is
collected to 15ml of the filtrate add 2 drops of phenolphthalein indicator and titrate against 3.1
normal Hcl. The pink colour is discharged and not more than 1 ml of Hcl is required.
Test for soluble salts
To 40ml of the above filtrate evaporate to dryness and dried mass ignited gently not more than 38 mg
of the residue should be obtained.
Acid absorption/ Acid neutralising capacity
The 0.3g of MgO3SiO3 is heated with 100ml of 0.05 N Hcl in a stoppered vessel and 37 oC for 3
hours. The solution is shaken for 30 second at 15 minute interval. The solution is then filtered and
cooled. Take 50ml of the above solution and titrate against 0.05N NaOH using methyl red as
indicator. 1g of the ignited substance required not less than 250ml of 0.05 N Hcl.
Ability of antacid to neutralise the Hcl neutralising capacity
Uses
It is used antacid
It uses gastric hyper acidity and pain associated with gastric and duodenal ulcer.
It is used a absorbent
The gelatinous mass forms a protective coating on GIT and adsorbent effect on the gastric
mucosa. Colloidal SiO2 protects from further acid and pepsin.
Pharmaceutical Chemistry-I
39
The acid neutralising capacity of an antacid is expressed in mille equivalence (mEq) of Hcl
Every antacid product must have total neutralising capacity of at least 5 mEq of Hcl per
dosage unit.
Very antacid must neutralise excess acid and arise the pH of empty stomach above 3.5.
Product Is more potent then it will neutralise more amount of acid.
If the product is neutralises 2.5mEq acid for those is half as potent as the one neutralises 5
mEq of acids.
The product which neutralises 10 mEq is wise as potent as the one neutralises 5 mEq.
ALUMINIUM HYDROXIDE
CHEMICAL FORMULA: Al (OH)3
Standard
It is white viscous suspension of hydrated Al oxide with varying amounts of basic
Aluminium carbonate. It contains not less than 47% o Aluminium oxide when ignited to a constant
weight.
Preparation
Aluminium hydroxide gel is prepared by adding a boil solution of potash alum. Slowly with constant
stirring to a hot solution of Na2CO3. After removal of Co2 the precipitate of Al (OH)3 is obtained. It is
washed with hot water and the precipitate is dissolved in distilled water to obtain the required
strength.
3 Na2Co3 + 2 KAl(So4)2 + 3H2O 3Na2So4 + K2So4+2Al(OH)3 + 3Co2
Properties
It is a white viscous suspension and a clear liquid separates out when kept to for several time.
It is an ideal buffer and can uses the pH from aluminium chloride
Al(OH)3 + 3 Hcl Alcl3 + 3H2O
Identification Test
Al(OH)3 in dilute Hcl gives the characteristic test for Al ions.
Test for purity
It is tested for alkalinity NH3 salt. Arsenic, cl sulphate and acid neutralising capacity.
Test for chloride
0.5g of the gel is dissolved in 5ml of dilute Hcl. Boil the solution and cool dilute the solution to
100ml with distilled water. Take 25ml of the diluted solution of the filtration and perform the lt test
for chloride.
test for sulphate
5g of the gel it dissolved in 5ml of dilute. HNO 3 acid. Heat the solution cool and dilute to 200ml with
water. The solution is mixed well. Collect the filtrate. Take 10ml of the filtrate and add 2ml of diluted
Hcl and carry out the lt test for sulphide.
pH
Equal volume of Al(OH)3 is diluted with distilled water the pH of the solution should not be more than
7.5.
Acid neutralising capacity / Acid absorption
An accurately weighed quantity of the gel (.5ml) is taken in a flask to it add 50ml of 0.1 N Hcl and
shake the contents of flask for one hour at 37 oC. Then the solution is titrated for excess of Hcl with
Pharmaceutical Chemistry-I
40
0.1 N NaOH using bromo phenol blue solution as indicator. 1g of the gel should neutralise not less
than 12.5 ml and not more than 25ml of 0.1N Hcl.
Assay
Complexometric back titration
Weigh accurately about 5g of Al(OH)3 taken in the flask and dissolving 3ml of dilute Hcls by
warming over water bath. Cool the solution and dilute to 100ml with distilled water. Take 20 ml of
above solution in a conical flask and add 40ml of 0.05M disodium EDTA and add 80ml of water and
neutralised with 1N NaOH solution using methyl red as indicator. Now the colour changes from red
to yellow. Warm in a water bath for half an hour and add 3g of hexamine. Titrate the excess amount
of 0.05m disodium EDTA against 0.05 m lead nitrate using xylenol orange as indicator. The end point
is appearance o violet colour. Each ml of 0.05m disodium EDTA is equivalent to 0.002549g of Al2O3.
Uses of Al(OH)3
It is used as antacid, in the treatment of hyperchlorbydria.
It is used for the treatment of intestinal toxaemia.
It is used for the treatment of hypo para thyrodism.
It is used for the treatment of peptic ulcer
It is used widely in combination antacid.
Storage
Stored in a well closed container, shake well before uses. Stored at temperature not exceeding 25C. It
should not be allowed to freeze.
Potassium citrate
Chemical formula:
Standard
It contains not less than 98% and not more than 100.0% of potassium citrate. Calculated with
reference to dried substance.
Preparation
Potassium citrate is prepared by neutralising citric acid with potassium carbonate of potassium
bicarbonate. The solution is evaporated to obtain crystal of potassium citrate.
Pharmaceutical Chemistry-I
41
Properties
White crystal line powder, odourless, having a cooling saline taste.
It is deliquescent in nature
It is soluble in water and glycerine and insoluble in alcohol.
On heating at high temperature, it gets converted to its carbonate form.
Identification tst
Aqueous solution of potassium citrate gives the characteristic test for potassium and citric acid.
Test for purity
It is tested for acidity and alkalinity. Cl, S, As, Fe heavy metals and loss on drying (LOD)
Uses
It is used as antacid
It is used as Anti-coagulant
It is used as osmotic diuretic
It is used as expectorant
It is used diaphoretic
It is used as systemic alkaliser
Storage
Stored in a well closed contained protected from moisture.
COMBINED ANTACID THERAPY
Antacids like calcium and aluminium salts after being converted to soluble salts by gastric acid
produces constipation effect.
The magnesium containing antacid produces laxative effect. Therefore its common to market a
constipating and laxative causing antacid in combination.
This will reduce the unwanted side effect of each o these antacids.
Eg: Megaldrate
MEGALDRATE
Al5Mg10(OH)31(SO4)2 .xH2O (Chemical formula)
Synonym
Hydrated magnesium aluminate
Standard
It is a chemical combination of aluminium hydroxide and magnsisium hydroxide along with
sulphates of aluminium and magnesium contains not less than 28-39 % of magnesium hydroxide and
not less than 25% of aluminium hydroxide.
Properties
It is the white crystalline odourless powder.
Insoluble in water and alcohol. Soluble in dilute solution of mineral acids.
It is having optimum acid neutralising capacity. It is superior to products of simple mixtures
of Aluminium hydroxide gel and magnesium hydroxide.
Test for purity
It is tested for Arsenic, heavy metals, soluble chloride, soluble sulphide, sodium aluminium
hydroxide, Magnesium hydroxide; sulphide ,microbial limits and lose on dying (LOD)
Pharmaceutical Chemistry-I
42
Test For soluble chlorides: A hot aqueous extract of the substance is titrate with 0.1m AgNO 3 using
potassium bromated as indicator.
Test for Soluble sulphates: To the aqueous extract add 2ml of dilute Hcl and 5ml Bacl2 solution .Any
turbidity produces; it should not be greater than 0.01M in H2SO4 treated in similar manner.
Uses
It is a combined antacid used for the treatment of peptic ulcer.
It is used for the treatment of gastritis.
Pharmaceutical Chemistry-I
43
Coarse Particles
Light Kaolin contains certain limit of coarse particles. The coarse particles larger than to micron
in diameter should not present. It is determined by preparing a suspension of the sample. In the
solution of sodium pyrophosphate and withdrawing after 5 minutes and aliquot of suspension
below 5c m of water has to been collected. The remainder is evaporated to dryness on a water
bath and the residue dried at 105oC and weighed the remainder of the suspension contain coarse
particles and its diameter is measured.
Soluble Matter
It is tested by boiling the sample with 02m Hcl and evaporating to a definite volume of the
filtrate, to dryness the residue is ignited at 600oC and weighed.
Loss on drying
Not less than 1.5%
Loss on ignition
Not more than 15%
Uses
Adsorb toxins in conditions like enteritis, colitis and dysenteric. It is used as protective
and adsorbents, conditions like food poisoning and alkaloid poisoning.
Topically it is used as dusting powder.
It is used as filtration aid
ACTIVATED CHARCOL
Preparation
It is obtained as a residue during destructive distillation of various organic matters or from burning of
organic material in a specified manner. The coarse material obtained is crush and finally powdered
the particles size is finally reduced to obtain activated charcoal.
Properties
Fine black odourless, tasteless powder having smooth touch and free from gritty particle
Insoluble in most of the solvents.
Identification test
On heating to redness it burns slowly without flame.
Test for purity
Acidity or alkalinity acid soluble substances ethanol soluble substances, alkali soluble substances,
coloured matter, chloride, sulphide, un carbonates constuents, Cu, Pb, Zn, sulphated ash, absorbing
powder and loss on drying.
Adsorbing powder
Activated means adsorption powder is increased by heating to a high temperature in a stream of gas
and co2. It should be not less than 40% of its on weight of phenazone. Shaken and filtered to the
filtrated containing an amount of phenazone not adsorbed by charcoal in 5% phenazone soln is added
to the sample. Shaken and filtered. To the filtrate containing an amount of phenazone Potassium
bromide and Hcl are added. The mixture is titrated with K-bromated solution . A blank is performed
from these. The percentage of phenazone adsorbed by charcoal is calculated.
Acidity and Alkalinity
It is determined by preparing a hot aqueous extract of the sample and filtering it. To the filtrated
bromo thymol blue solution is added and specific volume of 0.02mNaOH is added. The solution
Pharmaceutical Chemistry-I
44
turns to blue and not more than a specified volume of 0.02m Hcl is requires changing the colour to
yellow.
Un carbonates constituents
These are those natural sources that are not converted into charcoal. Alkaline extract of the sample is
filtered and filtrates should be colourless.
Alcohol and acid soluble substance
A hot aqueous extract is prepared in Hcl and the filtrate evaporated to dryness and weighed.
Uses
Properties
White of pale yellowish, odourless and tasteless powder.
It is insoluble in alcohol or water but dissolves with effervescence in dilute Hcl and dilute
HNo3.
It is stable in air and slowly gets decompose to Bismuth oxide upon ignition
Identification test
Pharmaceutical Chemistry-I
45
Bismuth carbonate treated with dilute Hcl treated with H2o. The white preparation of Bismuth oxy
chloride is obtained.
On passing H2s gas through a Hcl solution of Bismuth salt a brownish black precipitate of Bismuth
sulphide is obtained.
Test for purity
It is tested for clarity and colour of solution. Alkalinity and alkaline earth metals, arsenic, copper,
lead, silver, nitrate, sulphide, Nitrate, lose on drying and carbonate.
Carbonate: Impurity occurs due to incomplete washing and other impurities of alkali and alkaline
earth metals are tested.
Bismuth is removed as sulphide od treatment with dilute H2So4 . So it is evaporated to dryness and
the residue obtained should not be more than the prescribed limits.
Sulphide: It is detected by preparation with BaSO4 reagent.
Copper: It is detected by formation of blue colour with NH3 solution.
Uses
Storage
Stored in a well closed contained protected from moisture.
Anti Flatulent / Gastric deforming agent
Dimethicone / Semithicone
Synonym
Simethicone or activated dimethicone .[Poly dimethy Siloxane]
Standard
It is mixture of fully methylated linear siloxane polymer containing repeating units of (CH 3)2 SiO
with trimethyl siloxy (CH3)3 SiO end blocking units with finally divided SiO 2. It contains not less
than 90% and not more than 99% of ply dimethyl siloxane and not less than 4 and not more than 7%
of SiO2.
Preparation
Hydrolysis and poly condensation of Dichloro dimethyl silane and chloro trimethyl silane and chloro
trimethyl silane gives dimethicon
Properties
It is clear or translucent, colourless viscous liquid
The boiling point increases with the chain length of the compound , similarly the viscosity
increases the chain length of the compound.
It is stable to heat, it is having water repellent property which is due to the organic side chain.
Solubility
It is visible with carbon tetra chloride, chloroform, ether.
Pharmaceutical Chemistry-I
46
SALINE CATHARTICS
Purgatives or Laxatives
These are GIT agents that quicken or increase the evacuation of faecal matter from the bowl or
intestine. These agents enhance or promote the defecation process.
Deference between purgatives and laxatives
Purgatives
Laxatives
They produce strong action
Mild action
Elimination of soft but formed stools
More fluid evacuation
Large dose
Small dose
Conditions of uses of laxatives
1) To relieve acute constipation
2) To uses defecation in patience with painful haemorrhoids (Piles) or other rectful disorders.
3) Provide excessive staining and concurrent increase In abdominal pressure inpatients with
hernia.
4) Prevent harmful rise in BP during defecation in patients suffering from hyper tension, cerebral
coronary and other arterial diseases.
5) To remove solids materials from intestinal tract prior to surgery.
Constipation
It is infrequent or difficult evacuation of faecal matter.
Reasons
1) Person resisting the feeling or urge to defecate.
2) Intestinal spasm (Inflammation of intestine)
3) Emotional condition
4) Drugs
5) Diet
Types of laxative action
1) Stimulant laxative
2) Bulk forming laxative
3) Emollient laxative
4) Saline cathartics
Pharmaceutical Chemistry-I
47
Stimulant
They act by local irritation in the intestinal tract which leads to increase in peristaltic activity
causing evacuation of faecal matter.
Eg: castor oil, phenolphthalein, Aloin
Bulk forming
These agents swell on wetting leading to increased bulk in the bowel causing stimulation of
peristaltic movement leading to defecation
Eg: Methyl cellulose, Psllium seed, karaya gum
Emollient
They act as lubricants facilitating the passage of hard faecal matter. They act as stool softener.
Eg: mineral oil like liquid paraffin, d octilesodium sulfo succinate.
Saline cathartics
These agents quicken and increase evacuation of faecal matter from the intestine by increasing
the osmotic load of GIT.
These agents or salts of poorly absorbable unions and cations, it leads to hyper tonicity of gut. The
body overcomes this condition by secreting additional fluids into the intestinal tract by the osmotic
action. This results in increased bulk causing stimulation of peristaltic movement and leading to
evacuation of faecal matter.
Eg: Poorly absorbable anions
Biphosphate Phosphate
Sulphate
Tartarate
Eg: Poorly absorbable cations
Eg: Magnesium sulphate and Magnesium carbonate
Magnesium sulphate
Synonym: Epsom Salt
CF: MgSo4. 7H2o
Standard
Contains not less than 99& and not more than 101%.Calculated with reference to dried substance.
Preparation
1) By the action of dilute H2SO4 on Mg oxide . The solution obtained is filtrate the filtrate is
evaporated to obtain the crystals of MgSO4
2) When dolomite is passed into a solution of dilute H 2SO4 the sparingly soluble calcium
sulphate is removed the filtrate is collected and evaporated to obtain crystals of MgSO4
Properties
Colourless white crystalline powder having a efflorescence in warm dry air.
The aqueous solution is neutral to litmus.
Soluble in water sparingly soluble in alcohol
On heating at 200oC the MgSo4 uses water of crystallisation, on heating above 200 oC
oxidise is formed
Pharmaceutical Chemistry-I
48
Mg
It forms double salt with other sulphates like Na2SO4, KSO4, NH4So4 with a general formula
49
20. Write the preparation, assay & uses of aluminium hydroxide gel.
(5)
21. Write the preparation, assay & uses of aluminium phosphate
(5)
22. Write the preparation, assay & uses of magnesium hydroxide.
(5)
23. Write the preparation, assay & uses of Magnesium trisilicate
(5)
24. Write the preparation, assay & uses of light magnesium carbonate.
(5)
25. Write the preparation, assay & uses of heavy magnesium carbonate.
(5)
26. Write the preparation, assay & uses of calcium carbonate
(5)
27. Write the preparation, assay & uses of dimethicone
(5)
28. Write the preparation, assay & uses of megaldrate
(5)
29. Write the preparation, assay & uses of Bismuth carbonate
(5)
30. Explain the method of preparation, assay & uses of sodium bicarbonate & potassium citrate.
(10)
31. Explain the method of preparation, assay & uses of aluminium hydroxide gel & aluminium
phosphate.
(10)
32. Explain the method of preparation, assay & uses of magnesium hydroxide & magnesium
trisilicate.
(10)
33. Explain the method of preparation, assay & uses of light & heavy magnesium carbonate. Write a
note on the difference between them.
(10)
34. Explain the method of preparation, assay & uses of calcium carbonate & dimethicone. (10)
35. Explain the method of preparation, assay & uses of & Bismuth carbonate & magaldrate.(10)
(i) Acidifiers
1. Write a note on acidifiers.
2. Write the chemical formula uses of following compounds.
(i) Dil hydrochloric acid
(ii) Sodium phosphate
(iii) Ammonium chloride
3. Write the assay of ammonium chloride.
4. Write a note on method of preparation, assay & uses of sodium phosphate &
ammonium chloride.
(ii) Saline cathartics
(5)
(5)
(5)
(10)
Pharmaceutical Chemistry-I
50
(5)
(5)
(10)
Pharmaceutical Chemistry-I
51
B. TOPICAL AGENTS
TOPICAL AGENTS
These agents are used externally or topically to protect the skin surface. Treatment of skin disorders
and infestation and for relief of certain skin discomfort and related purpose. These agents are applied
on the skin or mucous or in body cavities (oral, vaginal and colorectal cavities),
Eg: protective, adsorbents, astringents and antimicrobial agents.
PROTECTIVES
These are inorganic agents applied on the skin surface to protect the skin from irritation due to
inflammation, allergies and friction of the skin surface.
Ideal properties of protectives
Insoluble in water, chemically inert.
They are fine particles.
High adsorbent property
Should not be applied on the skin surface which is broken, exuding fluid.
Eg: talc, Calamine, Zinc stearate, silicon polymer, dimethicone.
Talc
Synonym: talcum powder, purified talc, French chalk, soap stone.
Chemically it is hydrated magnesium silicate.
Chemical Formula
3MgO 4SiO2xH2O
Standard
Talc is a native of hydrated magnesium silicate containing a small proportion of aluminium silicate.
Preparation
It is obtained from native minerals. The minerals are finely powdered and treated with diluted Hcl. It
is washed thoroughly with water until it is free from acid. The dilute Hcl removes iron and other
impurities like Al2o3, calcium oxide and ferric oxide
Property
It is hydrated magnesium silicate contain 28.1 31.9% of MgO. 57-62% silicon dioxide and
3-7% water.
It is very fine powder white or greyish white.
Free form gritty particles.
Unctuous to touch.
Talc is smooth and greasy feeling to touch and in lump form is known as soap stone.
Unreactive to acids and bases.
Chemically inert to most of the reagent.
Odourless, tasteless, insoluble in H2O and dilute acids.
Neutral to litmus.
Test for purity
Tested for acidity and alkalinity, water soluble substance, acid soluble substance, iron, carbonate,
magnesium, chloride and loss on drying.
Uses
Used protective dusting powder.
Used as lubricating agent
Used to prevent irritation due to friction. Perfumed talc is used as cosmetic along with
antimicrobial agent like boric acid.
Pharmaceutical Chemistry-I
52
Property
Very fine, odourless, Amorphous, white powder, free from gritty particles.
Insoluble in H2O and alcohol
Adsorb Co2 from air to form Zinc carbonate
ZnO heated to 400oC 500oC. The oxides develops yellow colour which disappears on
cooling.
React with diluted Hcl to form Lewis acids.
ZnO+ 2Hcl Zncl2 + H2O
Zno react with ammonium hydroxide and NH4Co3 form water soluble basic ammonium
compound.
Pharmaceutical Chemistry-I
53
Pharmaceutical Chemistry-I
54
Properties
Fine white powder, free from gritty particles and has a faint characteristic odour due to the
presence of stearic acid. Unctuous to touch and readily adheres to the skin.
Insoluble in water, alcohol, ether
Gets hydrolysed in Hcl to form a soluble Zn salt (Zncl2) and insoluble oily layer of stearic
acid
Identification Test
Zn stearate is hydrolysed using diluted Hcl to form a lower aqueous layer of Zinc salt and upper layer
of oily insoluble stearic acid. The lower aqueous layer is neutralised and tested for Zinc salt.
Test for purity
Tested for alkali and alkaline earth metals, free fatty acids, arsenic, lead, chloride, sulphate, Co2
Test for alkali and alkaline and earth metals:
1g of Zinc stearate is dissolved in 25ml H 2O and add 5ml of diluted Hcl, Boil, filtered, washed with
hot water and add dilute NH3 solution to make the filtrate alkaline and add ammonium sulphide
solution to precipitate Zinc as ZnOH. Filter and add 5ml of dilute H 2So4 to the filtrate, evaporated to
dryness. The residue obtained not more than 20mg.
Test for free fatty acids
5g of Zinc stearate is shaken with 100ml ether. The mixture is filtered and 50ml of the mixture is
evaporated and weighed. The residue obtained should not be more than 50mg
Uses
Used as topical protective
protective as Dusting powder and Ointment
Mild astringent
Weak antimicrobial action
Used in various dermatological problem
Used for lubrication of granules in tablet manufacturing
Storage
Stored in well closed container.
Titanium dioxide
Chemical formula: TiO2
Standard: Contain not less than 98% not more than 101%.
Preparation
It is obtained from the natural ore ilmenite. Ferrous titanate obtained from ilmenite is treated with Hcl
and chlorine gas is passed. The precipitate obtained is filtered and washed and calcined to obtained
anhydrous oxide of titanium.
Properties
White powder, odourless, tasteless
Pharmaceutical Chemistry-I
55
TiO2 reacts with carbon and passing cl gas,, titanium tetra chloride is obtained.
Identification Test
TiO2 is dissolved in hot con H2So4 and on passing H2O2 solution orange red coloured solution of
titanium peroxide is formed.
Test for purity
It is tested for clarity and colour of solution, acidity and alkalinity, barium, heavy metals, water
soluble substances, acid soluble substances, Arsenic, lead, loss or drying.
Uses
Topical protective agent due to its high refractive index
Used protective in sunscreen product
5-25% TiO2 in ointment and lotions is Used as solar ray protective
Used as pharmaceutical aid in coating of tablets
Cosmetic preparation.
Storage
Stored in well closed container.
Silicon polymer
Dimethyl poly siloxane/ dimethicone/semithicone.
These are inert protective occurs in liquid form. Commonly known as silicon oil
Chemically it is dimethyl poly siloxane
Preparation
It is obtained by polymerisation reaction of dialky Silane diol
Properties
Colourless, odourless, highly viscous liquid.
Water repellent property
Practically insoluble in water
Miscible with organic solvents like benzene, ether, chloroform.
There are various grades of silicone polymer, dimethicone 20,200,350,5000 which are
soluble in amyl acetate, cyclohexane, diethyl ether
Silicon oil adheres very well to the skin and exclude contact with air for this reason they
should not be applied on broken skin. Contact with eyes should be avoided.
Viscosity of silicone polymer depends on molecular weight and cross linking of polymer.
These are highly stable compound chemically and biologically inactive fluids and are able to
with stand at high temperature.
These liquid has low surface tension, thermostable, they are resistant to most of the chemical
substances but affected with strong acids.
Uses
Topical Protective
Pharmaceutical Chemistry-I
56
Properties
Colourless, odourless, transparent crystals, having sweetish astringent taste.
Soluble in cold water and glycerol. But more soluble in hot water.
Practically insoluble in alcohol
Solution of alum is acidic in nature.
10% solution of alum has a PH between 3-3.5
When it is heated it melts at 92oC and looses all water molecules
At 200oC becomes anhydrous leaving a white residue known as burnt alum containing
aluminium and potassium sulphate.
Identification test
The aqueous solution of alum gives characteristic test for K, Al, sulphate
Test for purity
It is tested for arsenic, iron, Zn, ammonium salt and loss on drying.
Test for Zn
Pharmaceutical Chemistry-I
57
Identification Test
ZnSO4 reacts with H2S to form a ppt of ZnS. It is insoluble dil acetic acid and soluble in dil Hcl.
ZnSO4 results with potassium ferrocyanide solution to form white ppt of Zinc ferrocyanide which is
insoluble in dil Hcl.
Pharmaceutical Chemistry-I
58
Assay of Zncl2
Complexometric titration
An accurately weighed amount of Zncl2 is dissolved in distilled water. 10ml of ammonia ammonium
chloride buffer (pH 10) is added. 10mg of mordant blank II or solo chrome blank T used as
indicator. The solution is titrated against .05M disodium EDTA. The end point is colour change from
wine red to blue colour.
Uses
Powerful astringent.
Mild antiseptic due to interaction of Zn with the enzymes of microbes.
Preparation of mouth washes and deodorant.
Pharmaceutical Chemistry-I
59
Antimicrobial agents
These are inorganic agents used to kill or inhibit the growth of micro organism in either living or non
living organism. The term antimicrobial agents includes antiseptics germicide, disinfectant and
sterilization
Anti septic
These agents are used to kill or inhibit the growth of microorganism (Bacteria, fungi) in animate
object, living organism) e.g.: KMnO4,I2, H2O2, boric acid
Germicide (Cide=kill)
These agents are used to kill the micro organism and it includes bactericide, fungicide
Disinfectants
These agents are used to kill or inhibit the growth of microorganism especially inanimate objects
(non living organisms) e.g.: bleaching powder.
Sterilization
It is the process to render on object completely free from microorganism. It involves the uses of
chemicals or mechanical means like applying heat and radiation.
Mechanism of antimicrobial action
Oxidation
The various chemicals used include hydrogen peroxide, metal peroxide, permanganates and
halogens. These agents cause oxidation of reducing groups like sulphidal group present in proteins. It
leads to the formation of disulphide bond or bridge. This leads to change in conformation of proteins.
It will ultimately lead to inhibitor or destruction of microorganism.
Halogenation
This mechanism includes the uses of chemical like hypochlorite, oxy hypochlorite. These agents
causes halogenation of peptide linkage of protein molecule. It leads to change in conformation of
protein Becauses of non formation of hydrogen bonding. It will ultimately lead to inhibition or
destruction of microorganism.
Protein precipitation
There are metallic ions like copper, aluminium, zinc which has large charge per radius ratio or strong
electrostatic fields forms complex with various polar groups in the protein. The protein acts as ligand
and form complex with metal ions leading to protein precipitation.
Hydrogen peroxide
Chemical formula: H2O2
Standard: Contains not less than 5% W/V not more than 7% W/v corresponding to 20 volume or
available oxygen. (H2O2 20 volume)
H2O2 100 volume contains not less than 26% w/v nor more than 28% w/v H2O2 corresponding to 100
volume O2
Preparation
Decomposition of barium oxide using phosphoric acid gives hydrogen peroxide.
Pharmaceutical Chemistry-I
60
Thin paste of barium oxide in cold water is gradually added to ice cold con. H2SO4 when the
reaction mixture is slightly alkaline to the add H2So4 to make acidic to litmus, is then
cooled and insoluble BaSO4 is filtered.
By electrolysis of H2SO4 gives per sulphuric acid which on distillation gives hydrogen
peroxide.
Property
Clear, colourless, odourless liquid. It decomposes rapidly on heating.
Stabilised by adding stabilizing agents like boric acid and urea
It forms addition compounds with organic compound like urea to urea peroxide
Identification Test
H2O2 solutions are made alkaline and heated and get decomposed with effervescence
evolving oxygen.
To 1ml of H2O2 add 20ml of water and a drop of potassium bromide solution and 2ml of other
solution. The other solution becomes blue in colour.
Test for purity
It is tested for acidity and alkalinity preservatives, barium, non volatile melter and lose of
evaporation.
Test for acidity
Pharmaceutical Chemistry-I
61
To 10ml of H2O2 add 20ml of water. Titrated against .IN NaOH using methyl red as indicator. The
end point is the appearance of pink colour. The limit test not less than .2ml not more than 1ml of
NaOH required to produced pink colour.
Preservatives
100ml of H2O2 is treated with 3 part of chloroform and 2 parts of solvent ether. The solvent is
evaporated the residue should not be more than 50mg.
Test for barium
To 2ml of H2O2 add 1ml of dilute H2SO4 and should not produced any turbidity.
loss on evaporation
The H2O2 heated on a water bath and the residue should not be more than 0.2%
Non volatile matter
By evaporating H2O2 solution on a water bath dry the residue at 105oC and weigh.
Assay
Oxidation reduction method (Redox titration)
H2O2 reduces KmnO4 in presence of dilute H2SO4.
To 10ml of H2O2 is diluted to 50ml with distilled water and add 10 ml of 5N H 2SO4. Titrated
against .IN KmnO4. The end point is appearance of faint pink colour. KmnO 4 act as self indicator.
Each ml of .IN KmnO4 is equivalent to .001701g of H2O2.
Uses
Used as mild oxidising and antiseptic agent
It kills most pathogenic bacteria like e.coli, staphylococci aureus and typhoid bacilli.
Used for cleaning of ear canal
Used in removal of dirt, bacteria, debris from the surface of wound.
Used in mouth washes for treatment of bacterial infections of throat and mouth.
Bleaching of hair.
Storage
Stored in light resistant container in a cool place. Stored only in glass bottle and cock. Rubber or
metal should not be used for storing. Since it will attack them. Not stored for long period.
POTASSIUM PERMANGANATE
Chemical formula: KmnO4
Standard: Contain not less than 99% not more than 100.5% KmnO4
Preparation
Mangnese dioxide is fused with excess of KOH in presence of oxidising agent like potassium
chloride. A green residue of potassium manganate is obtained. It is further oxidised using
chlorin or Co2 to give KmnO4.
Large scale method: Potassium manganate undergo electrolysis using Ni anode and iron
cathode to obtain KmnO4
Pharmaceutical Chemistry-I
62
Properties
Dark purple coloured crystalline compound having a metallic luster.
It is odourless soluble in 3.5 parts of boiling water and 15 parts of water
Kmno4 get decomposed at high temperature
Identification test
Potassium permanganate is dissolved in dilute H 2SO4 and heated with H2O2 solution. The
solution get decolorized.
KmnO4 is dissolved in water and heated a black residue of manganese dioxide is formed and
the solution give the characteristic test for potassium.
Test for purity
Pharmaceutical Chemistry-I
63
It is tested for chloride, sulphate, sulphide and water insoluble matter. The L.T is performed after
decolourising KmnO4 with alcohol.
Uses
Oxidising, antiseptic agent
Used as an antiseptic in mouth washes, cleaning of wounds.
Used as antibacterial and anti fungal agent.
It oxidises snake venom present in the skin surface.
It is also used as disinfectant agent.
Storage
Stored in a tightly closed container. It can explode on contact with oxidising substances.
Boric Acid
Chemical formula: H3BO3
Standard: It contain not less than 99% not more than 100.5% of boric acid calculated with reference
to dried substance
Preparation
Decomposition of borax using sulphuric acid by adding a mixture of con H 2 SO4 and water to
a boiling solution of borax. The hot liquid is filtered the liquid on evaporation yield crystals of
boric
acid.
Industrial Method: On passing SO2 gas in to finely powdered or colemanite, boric acid
obtained.
Properties
White, triclinic crystals, odourless
Soluble in water, alcohols
Boric acid on heating at 100oC forms metaboric acid on further heating. It is converted to
tetraboric acid and on heating above 100oc forms borontrioxide.
Boric acids react with sodium hydroxide form sodium meta borate.
Identification Test
To boric acid solutions add alcohol heat it on a flame the flam turns green due to the formation of
ethyl borate.
Pharmaceutical Chemistry-I
64
Uses
Storage
Stored in a well closed container
Silver nitrate
Chemical formula: AgNo3
Standard: Not less than 99% not more than 101% of silver nitrate.
Preparation
By the action of hot concentrated nitric acid on silver metal. The solution is heated to dryness
to obtain crystals of AgNo3
Properties
White crystalline powder, odourless and tasteless.
Freely soluble in water and ethanol
Very slightly soluble in ether and glycerol
On heating AgNo3 get converted to silver nitrate and on red hot heating silver metal is
deposited
Pharmaceutical Chemistry-I
65
Identification test
AgNo3 reacts with ammonium thiocyanate to form reddish yellow precipitate of silver thiocyanate.
Test for purity
It is tested for acidity, alkalinity, clarity and colours of solution, Ai, Bi, Cu, Pb, foreign salt and loss
on drying.
Acidity and alkanity
Prepare 4% AgNo3 solution. To one part of the solution add Bromocresol green solution. A blue
colour is obtained. To another part of the solution, phenol red is added the colour of the solution is
yellow. Testing should be done in PH 5.2 -.6.8
Clarity and colour of solution
To 1g of AgNo3 add a mixture of 6ml of H2O and 4 ml of strong ammonia solution. The resulting
solution should be clear.
Al, Bi,Cu,Pb
Precipitated with hydroxide, where AgNo3 remains dissolved in it .If Cu is present, it will produce a
blue colour due to the formation of Cuoxam.
Uses
Bactericidal agent
Used as astringent
Used to remove warts and other small skin growths
Used in eye drops for ophthalmic infections
Used in burn infections and irrigation fluids
Prolonged uses of silver preparations results in darkening of skin due to the deposition of
silver under epidermis. This conditions is known arggyria
Storage
Stored in light resistant tightly closed containers
Chlorinated lime/ Bleaching powder/ Calcium hypochlorite/ chloride of lime/calcium
oxichloride
Chemical formula: Ca(OCl)Cl
Standard: Contains not less than 30% w/v of available chlorine.
Preparation
By passing cl gas over slaked lime in the lead chamber for 8-24 hour. During this process
Ca(OH )2gets saturated with cl gas form calcium oxychloride. The temperature is maintained
below 25oC
.
Properties
Dry, dull, white or greyish white granular powder.
It has characteristic odour of chlorine.
Consist of calcium chlorohypochlorite which is intermediate between calcium chloride and
calcium oxychloride.
On prolonged exposure to air it gets decomposed with the liberation of chlorine gas.
Pharmaceutical Chemistry-I
66
Identification test
It is dissolved in Dil HCl/ dil. Acetic acid with liberation of chlorine gas.
Test for purity
It is tested for chloride, sulphate, calcium, led, heavy metals and loss on drying.
Uses
Storage
Stored in a tight resistant container and protect from moisture.
Selinium sulphide
Chemical formula: SeS2
Standard: Contains not less than 52% and more than 55% of selenium
Preparation
By passing H2S gas into selenieous acid solution to for selenium sulphide.
Properties
Bright orange powder with a faint odour.
Practically insoluble in water and organic solvent.
Dissolves in nitric acid to form selenious acid
Pharmaceutical Chemistry-I
67
Uses
Zinc undecenoate
Chemical formula:
Standard: Contains not less than 98% not more than 101%
Preparation
Undecenoic acid reacts with sodium hydroxide solution resulting in the formation of sodium
undecenoate.
Further result with ZnSo4 to form zinc undeceneate
Pharmaceutical Chemistry-I
68
Pharmaceutical Chemistry-I
69
(5)
(5)
(5)
(5)
(5)
Pharmaceutical Chemistry-I
70
c. DENTAL PRODUCTS
DENTAL PRODUCTS
These are large number of inorganic chemicals and their preparations used for dental and oral
disorders. These products includes tooth paste, tooth powder, mouth washes and rinses and tooth ache
drops, dental adhesives, denture cleaners. Dental products are mainly used for polishing, cleaning and
as anticaries agents
Role of fluride as anticaries agents
Indigenous bacterial floras present in the mouth are supposed to causes dental caries or tooth decay.
They act upon remaining food materials especially on sugars present on or between teeth cavities.
The bacteria act upon these foods releases acid (Lactic acid) during the process. The acid causes the
dissolution of minerals in enamel causing tooth decay or lesions within the teeth.
Fluoride ion produces anti caries action by the following mechanism. Fluoride ion decreases acid
solubility of enamel by forming a bond with the enamel and makes it tough agents against dental
caries. It also reduces number of defect in hydroxyapatite or by combining with carbonate during
apatite formation.
Fluoride also inhibits bacterial enzymes needed for their replication.
Administration of fluorides
Oral/ systemic
Here by fluoridation process: (By adding sodium fluride or fluro gives a fluride concentration of .7 to
1ppm. It gives 2.2 mg of sodium fluorides for a person taking 6 glass of water. Excess amount of
fluorine leads to Dental flurosis.
Topical
Topical fluorides present in tooth pastes, mouth washes and gells are less effective than systemic
fluorides such as fluoride in water supply.
Anticaries agents:
The inorganic agents which prevents tooth decay. (Caries means tooth decay)
Eg: NaF, sodium mono fluro phosphate.
Sodium fluoride
Chemical formula: NaF
Standard: Contain not less than 98% and not more than 100.5%
Preparation:
By neutralising hydrofluoric acid and with sodium carbonate sodium fluride is obtain.
Double decomposition of calcium fluoride with Na2CO3 the insoluble CaCo3 is removed by filtration
the solution Concentrated to obtain the crystal of NaF.
CaF2+Na2Co3 2NaF +CaCo3
Properties
White powder colourless, crystals, soluble in water, practically insoluble in alcohol.
On hydrolysis of NaF in an aqueous solution gives hydrofluoric acid.
NaF forms stable complex with iron compound like ferric chloride.
Pharmaceutical Chemistry-I
71
Identification test
NaF is dissolved in water and ad CaCl2. A white precipitate of calcium fluride is formed . It dissolves
by adding ferric chloride solution.
The aqueous solution gives characteristic test for sodium.
Test for Purity
It is tested for acidity and alkalinity clarity and colour of the solution, chloride, sulphate fluorosilicate
and loss on drying.
Assay
Non aqueous titration
The NaF is dissolved in acetic anhydride and glacial acetic acid by heating and cooled. It is titrated
against 0.1M perchloric acid. (HCl04) using crystal violet as indicator. The end point is the
appearance of green colour. A blank titration is also performed.
Uses
Used as anticaries agent
Used to prevent and inhibit tooth decay.
It is widely used in dental preparations.
Forms a bond with tooth enamel and makes it tough and strong.
Storage
Stored in a well closed container protected from moisture.
Dentrifices
These are inorganic agents used for cleaning and polishing of the teeth by its abrasive property.
Eg: Calcium carbonate
Dibasic calcium phosphate
ZnCl2
Dentifrices containing anti caries agents are wildly used in tooth paste and tooth powder.
Ideal properties of dentifrices
Should have abrasive property
Should have cleaning and polishing property
Should produce foam
Should have humectants
Dibasic Calcium phosphate
Chemical form: CaHPO4 2H2o
Standard: Contains not less than 98% and not more than 101% dehydrate salt at calcium phosphate.
Preparation
It is prepared by interaction of neutral solution of calcium chloride with disodium hydrogen
phosphate.
The solution is made neutral by the addition of alkali and the tribasic calcium phosphate formed is a
white precipitate of dibasic calcium phosphate is filtered and dried.
By the addition of phosphoric acid to calcium hydroxide solution a white precipitate of dibasic
calcium phosphate is obtained.
Properties
White crystalline powder, odourless, having a saline taste.
Pharmaceutical Chemistry-I
72
Identification test
A solution of dibasic acid phosphate in diluted HNO 3 gives characteristic test for calcium and
phosphate
Test for purity
It is tested for acid insoluble substances Ba, Carbonate, iron, Chloride sulphide, arsenic, heavy
metals, nitrate, reducing substances impurities.
Monobasic calcium and tri basic calcium
Test carbonate
By adding an aqueous solution of Hcl no effervescence is produced.
Test for barium: To aqueous solution of sample add diluted H 2So4 the solution should not be more
opalescence then a standard treated similarly.
Test for reducing substance: By acidifying with diluted H2So4 and add O.1 KMnO4 the pink colour
of the solution should not be discharged. It compared with standard of CaCo3 Similarly treated.
Monobasic and tribasic calcium phosphate: These are limited by dissolving the sample in diluted
Hcl and titrated with 1M NaOH using methyl orange as indicator.
Uses
Used as dentifrice in tooth paste and tooth powder.
Used as cleaning and polishing agent
Used as electrolyte replenisher
Used in the deficiency of calcium and phosphate
Storage
Stored in a well closed container, protected from moisture
Zinc chloride
Chemical formula: Zncl2
Standard: it contains not less than 98% - not more than 101% of Zncl 2 calculated with reference to
dried substance
Preparation
Prepared by reacting metallic Zinc and Hcl the solution is evaporated to obtain crystal of
Zncl2.
By reacting ZnCo3 with hydrochloride acid Zncl2 is obtained.
Properties
White, crystalline powder, odourless, deliquescent in nature.
Freely soluble in water, alcohol, glycerine.
Aqueous solution is acidic in nature.
Zncl2 is hydrolysed to form hydrochloric acid and basic Zinc chloride
Identification test
The aqueous solution of Zncl2 gives the characteristic of Zn chloride
Test for purity
It is tested for acidity and alkalinity clarity and colour of solution, chloride, sulphate arsenic, heavy
metals and loss on drying
Pharmaceutical Chemistry-I
73
Uses
Used as dentifrice
Used in deficiency of the Zinc
Used as electrolyte replenisher
Astringent
Storage
Stored in well closed in well closed container, protecting from moisture, since it is deliquescent and
absorbs Co2
Model question Chapter wise
1. Explain the use of fluoride as anticaries agents
(5)
2. Define the following terms with examples
(5)
(a) Anticaries agents (b) De-sensitizing agents
(c) Dentifrices
3. Write the preparation & uses of sodium fluoride
(5)
4. Write the preparation & uses of dibasic calcium phosphate
(5)
5. Write the preparation & uses of strontium chloride
(5)
6. Write the preparation & uses of zinc chloride
(5)
7. Write the mechanism of action of fluoride as anticaries agents
(5)
8. Write the preparation, assay & uses of sodium fluoride
(5)
9. Write the preparation, assay & uses of dibasic calcium phosphate
(5)
10. Write the preparation, assay & uses of zinc chloride
(5)
11. Write the preparation, test for purity, assay & uses of sodium fluoride & zinc chloride.(10)
12. Write the preparation, test for purity, assay & uses of dibasic calcium phosphate & zinc chloride.
(10)
Pharmaceutical Chemistry-I
74
These 2 compartments are separated by a membrane which is permeable to water, inorganic ions like
Na, K chloride ions and organic compounds. The membrane is impermeable to macromolecule like
protein.
Each fluid compartment has distinct solute pattern. The solutions in each compartment are ionically
balanced. Na , ions, chloride ions are present in the interstitial and plasma fluid. K, Mg ions and
phosphate are present in intracellular fluid. The concentration of cations and anions in the plasma
fluid helps to maintain the osmotic pressure. The protein helps to maintain the oncotic pressure |(67g/100ml) . The electrolyte balance of the body is disturbed due to vomiting, diarrhoea, and
haemorrhage.
The following condition leads to electrolyte imbalance.
1. Loss of Na ions and water in the body (Hyponatremia)
It is treated by administering 9% sodium chloride injection to restore the extracellular fluid
volume.
2. Loss of water and excess Na ions (Hypernatremia)
It is associated with reduce intake of water or unusual water loss which leads to increase in
osmotic pressure ICF and ECF . It is treated by administering 5% dextrose injection.
3. Accumulation of excess fluid in the interstitial space with salt retention leads to enema. It is
seen in conditions like congestive heart failure and kidney failure. It is treated by giving
diuretics.
Fluid electrolyte concentration and composition inside the body
Srl.N Cations
Plasma fluid
Interstitial
ICF
o
Fluid
1
Na Ions
142
145 Eq/L
10.mEq/L
milliequalence/L
2
K ions
4mEq/L
4mEq/L
160mEq/L
3
Ca ions
5mEq/L
3mEq/L
Nil
4
Mg ions
3mEq/L
2mEq/L
35mEq/L
Total
154mEq/L
154
205mEq/L
Pharmaceutical Chemistry-I
75
ANIONS
1
Bicarbonate
2
Chloride ion
3
Phosphate
4
Sulphate
5
Organic acid
6
Proteins
Total
27mEq/L
103mEq/L
2mEq/L
1mEq/L
5mEq/L
16mEq/L
154mEq/L
30mEq/L
115mEq/L
2mEq/L
1mEq/L
5mEq/L
1mEq/L
154mEq/L
8mEq/L
2mEq/L
140mEq/L
Nil
Nil
55mEq/L
205mEq/L
76
Absorption
The dihydrogen phosphate anion (H2Po4) is completely absorbed from the intestine.
Requirements
The normal plasma concentration of phosphate is 1.7-2.6 mEq/L
Disorders
The excess of phosphate in blood leads to hyper phosphate. The serum phosphate level is co related
with serum Ca Level. When Ca conc is high it will lead to high phosphate level leading to hyper
phosphatemia. It occurs in conditions like hyppervitaminosis D, renal failure and hypothyroidism.
The excess phosphate gets deposited kidney leading to the formation of phosphatic urinary calculi.
Hyper phosphatemia is treated by administering basic aluminium carbonate.
Fefficiency
Decrease in phosphate serum blood conc. Leads to hypophosphatemia. It occurs in conditions like
vitamin D deficiency. Dercrease in Ca ion absorption and hyper parathyroidism. This condition is
treated by giving aluminium hydroxide gel.
PHYSIOLOGICAL ROLE OF BICARBONATE
Physiological function
It is the second most prevalent or present anion in ECF compartment. It is bony important
buffer system.
It is necessary to maintain the acid base balance inside the body.
To maintain hydration and osmotic pressure.
Disorders
Deficiency of bicarbonate leads to metabolic acidosis.
The excess of bicarbonate leads metabolic alkalosis.
PHYSIOLOGICAL ROLE OF SODIUM
Physiological functions
Sodium is a principle cation in the ECF compartment
It is necessary to maintain the acid base equilibrium condition in the body
It is responsible for maintaining the normal hydration and osmotic pressure in the body
It is essential to maintain the normal irritability of muscles and permeability of ions.
It is necessary for Co2 transport.
It is necessary the transmission of nerve impulse across the nerve fibres.
Absorption
It is completely absorbed from the GIT and reabsorbed from the glomerular regions of kidney.
Requirement
Normal plasma conc. Of sodium is 135-142mEq/L daily dietary requirements about 3-5g
Disorders
Deficiency: Decrease in serum conc. Of sodium leads to hyponatrimia. This condition occurs
due to metabolic acidosis, diabetes insipidus, Addisons disease diarrhoea and vomiting and
kidney failure.
Hyper natremia Increase in serum sodium occurs in conditions like severe dehydration,
hyper adrenalism, and excessive treatment with sodium salt.
PHYSIOLOGICAL ROLE OF POTASSIUM
Physiological function
It is intracellular cation present 23 times more than conc. Of potassium ion in ECF
compartment.
It helps in the transmission of nerve impulse by active transport mechanism called as sodium
potassium pump where sodium enters the cell and potassium leaves the cells.
It helps in the contraction of smooth muscles especially cardiac muscle.
Pharmaceutical Chemistry-I
77
To maintain the electrolyte composition of various body fluids and maintains the osmotic
pressure.
It helps to maintain various biochemical activities inside the cell
It helps to regulate the acid base balance by regulating the pH by exchanging with proton.
Absorption
Rapidly serum potassium concentration is 3.6-5mEq/L. Daily dietary requirement 1.5-4.5g
Disorders
Deficiency: Hypokalaemia
Decrease in serum potassium ion concentration occurs in the following conditions. Vomiting,
diarrhoea, haemorrhage, diabetic coma burns excess uses of thiazide diuretics and alkalosis.
Hyper Kalemia: The increase in serum potassium ion concentration occurs in condition like renal
damage acidosis and cardiac arrest. It is treated by administering calcium gluconate injection.
Physiological functions of Ca
Calcium is an essential ion present in the body. It is present 99% in bones and 1% in plasma.
Calcium is needed for bone formation and development.
Calcium in the bone is stored as hydroxyapatite.
The ionic plasma calcium is essential for neurohumoral function.
Ionic calcium is essential for blood clothing
Ionic calcium is essential for muscle contraction
Calcium ion is essential for release of neurotransmitter acetyl choline from preganglionic
nerve endings.
Absorption
Calcium ion is absorbed in the intestine.
Absorption of calcium is controlled by parathyroid hormone and dihydroxy cholicalciferol.
It also influence by serum phosphate ion.
Requirements
The normal calcium ion concentration in plasma 2.2-2.6mEq/L
The daily requirement of calcium is 800mg.
Disorders
Hypocalcaemia
The decrease in serum calcium level leads to hypocalcaemia which is seen in conditions like hypoparathyroidism, vitamin D deficiency then bone cancer, Cushing syndrome, acute pancreatitis,
osteoporosis, Paget disease. It is due the inhibition of calcium metabolism which leads to
decalcification and softening of bones. It is treated by giving phosphate salt and calcitonin
hypercalcemia- in conc of ca in blood leads to hypercalcimia. It occurs in condition like bone cancer,
hyper parrathyroidism, hyper vitaminosis D. This condition is treated by administration of
phosphorus salt.
PHYSIOLOGICAL ROLE OF MAGNESIUM
Physiological functions
Mg is the second most abundant cation present in ECF compartment.
50% of Mg is combined with calcium and P involved in phosphate metabolism.
It is very essential for the enzymes involved in phosphate metabolism.
It is also required for ATP formation
It is essential for protein synthesis
It is essential for smooth muscle functioning of the neuro muscular system.
It also plays a vital role in carbohydrate metabolism
Pharmaceutical Chemistry-I
78
Properties:
It is a white crystalline colourless powder.
Odourless, saline taste and stable in air
Freely soluble i9n water, practically in alcohol and ether It reacts with silver nitrate to form
opalescence of silver chloride
Identification test:
The aq. Solution of Kcl gives the characteristic test for potassium chloride ion
Test for purity:
It is tested for acidity and alkalinity, clarity and colour of solution, bromides, heavy metals, as, Bu,
Fe, Mg, Ca and loss on drying.
Test for acidity and alkalinity:
1g of Kcl is dissolved in 10ml of water titrate the solution against N/100 Hcl using phenol red as
indicator. Not more than 6ml; of the acid or alkali is required to produce a colour change.
Test for Ca and Mg:
It is tested by dissolving Kcl in dilute NH3 solution and sodium phosphate solution the solution
should remain clear.
Test for barium:
1g of Kcl add 20ml of water filter the solution divide the solution into 2 equal parts. T one part of the
solution add 2ml of dilute H2So4 and to the other part of the solution add 2ml of water both the
solution should remain clear for 2 hours
Test for Iodine:
It is tested by adding to an aqueous solution Kcl No blue colour is produced.
Pharmaceutical Chemistry-I
79
Chemical properties
It gives white opalescence with AgNo3 solution to form Agcl
This ppt soluble in dilute NH3 solution and insoluble in dil. NO3
Nacl reacts with H2SO4 ,hcl or phosphoric acid to form salt
Pharmaceutical Chemistry-I
80
Identification test
Aqueous solution of Nacl gives the characteristic test for sodium and chloride ions
Test for purity
It is tested for acidity and alkalinity, ca, Mg, As,, Barium, iodide, Fe, heavy metals and loss o n
drying
Test for Ca and Mg
It is determined by complexometry titration by using disodium EDTA and mordant black 2 as
indicator.
Test for bromide and iodide
Same as Kcl
Uses
It is used as fluid and electrolyte replenisher.
It is used for preparation of normal saline
It is used for preparation of ringer solution and ringer injection.
Isotonic solution Nacl is used for wet dressing wounds
It is also used for irrigation of body fluids and tissues.
Storage
Since it is slightly hygroscopic cue to the small amount of Magnesium chloride and Cacl 2 stored in
tightly containers
Official solution of Nacl
Isotonic Nacl injection or normal saline. It is a sterile isotonic solution of Nacl in water for
injection. It contains 0.9% w/v of Nacl which contains 150 millimoles of sodium and chloride
ions.
Hyper tonic Nacl solution or hypertonic saline. It is a sterile solution of containing 1.6w/v
of Nacl. It gives 270 mmoles of sodium and chloride ions.
Compound sodium chloride solution (Ringer solution). It contains 0.86% of Nacl, 0.05%
Kcl, 0.33% sodium 4mEq/L potassium, 4.5mEq/L of calcium and 156mEq/L of chloride ions.
Sodium chloride and dextrose injection. It contain 0.11-0.45 of sodium chloride and 2.5% 5% of dextrose in water for injection
The above solution is used as fluid and electrolyte replenisher and irrigation fluid.
Calcium Replacement
Calcium Chloride
CF: Cacl2 02H2O
Standard: It contains not less than 98% and not more than 101% of Cacl 2 Calculated with reference
to dried substances.
Preparation
By adding a slight excess of pure Caco3 to a hot solution of dil Hcl. Filter the solution when the
effervescence stop evaporate the syrupy solution to form crystals below 10oC. An heating at 200oC
the hexahydride form of calcium chloride gets converted to dihydride form of calcium chloride.
Properties
Pharmaceutical Chemistry-I
81
Properties
White crystalline, odourless and tasteless powder
Stable in air
It gets decompose on heating above 100oC
Soluble in hot water freely soluble in cold water, insoluble in alcohol, ether and chloroform.
Gets decompose by mineral acids to form gluconic acid which on further dehydration forms
D- gluconolactone.
Pharmaceutical Chemistry-I
82
Identification Test
Calcium gluconate is dissolved in water and a solution of ferric chloride is added to form yellow
colour
Test for purity
It is tested for clarity and colour of solution, acidity and alkalinity, sucrose and reducing sugar,
chloride sulphate, heavy metals, As and loss or drying
Test for sucrose and reducing sugar
To a boiling solution of calcium gloconate and dilute Hcl and potassium cupric tartarate solution. No
ppt should be obtained.
Assay
Complexometry titration
To an accurately weighed amount of calcium glucomate dissolve in warm water add a known amount
of 0.05M< Mgso4 solution and strong NH3-NH4cl buffer (pH10). Titrate the solution against 0.05M
disodium EDTA using mordant black 2 as indicator, the end point is colour change from wine red to
blue colour. The blank titration is perfomrmed by taking only a definite quantity of 0.05M MgSo 4
solution
Uses
Pharmaceutical Chemistry-I
83
Properties
White odourless, tasteless granular powder.
It is soluble in cold water and readily soluble in hot water insoluble in ether and chloroform.
When heated above 120oC it loses water molecule and becomes anhydrous.
84
Properties
White colourless, tasteless, powder stable in air
It is insoluble in alcohol and almost insoluble in water
Dissolves readily in dilute acids like dilute Hcl and dilute HNo3
Identification Test
The substance dissolved in dilute Hcl which gives test for calcium and phosphate.
Test for purity
It is tested for chloride, sulphate, carbonate, Fe, As heavy metals and loss on drying.
Uses
It is used as fluid ant electrolyte replenisher .
It is used as replacement therapy for calcium and phosphorus
It is used as pharmaceutical aid especially as diluents
It is also used as antacid
Phosphate anion can neutralise two equivalent of gastric Hcl
Storage
Stored in a well closed container protected from moisture
PHYSIOLOGICAL ACID BASE BALACNE AND ITS IMPORTANT
The body produces acids from carbonic acid.(From Co 2 and lactic acid from metabolism). The
body maintains the physiological acid base balance ie. The physiological p H of the body ie, 7.38-7.42
due to the various metabolic reactions occurring in the body with in this PH ranges.
Normal PH range of some of the body fluids,
blood, 7.4-7.8, gastric juice 1.5 1.8 salvia 6.4 7.4 , gall bladder bile 5.5-7.7, duodenal fluid, 5.57.4, pancreatic juice 7.5-8.2, urine 4.5-8.
The physiological acid base balance is maintained by 3 main buffer systems present in the body
1) Bicarbonate carbonic acid buffer system (HCO-3/H2Co3)
This is present in plasma and kidney
2) Phosphate buffer system
Monohydrogen phosphate and dihydrogen phosphate (HPO42-)
This buffer system is present in cells and kidney
3) Haemoglobin buffer system
It is present in RBC. It is the most effective single buffer system for buffering the carbonic
acid produced during metabolic reaction in the body
4) Bicarbonate carbonic acid buffer system
This buffer system is necessary for exchange of Co2 produced in lungs, plasma and tissues for
oxygenation.
Co2 reacts with water in presence of carbonic anhydrase enzyme at plasma level to form
carbonic acid
The plasma proteins act as buffer which decrease the PH value due to the formation of
Pharmaceutical Chemistry-I
85
carbonic acid. The oxyhaemoglobin of erythrocytes activates the bicarbonate anion causing
diffusion of RBC from the cell and chloride ion diffuses into the cells. This is called as
chloride shift.
The above reaction is reversed in the lungs where Hb gets oxidise to oxyhacmoglobin and
bicarbonate anion expels the co2 form the body
6) The steps involved in the excretion of the acid from the body are,
1) Sodium salt of organic and mineral acids are removed from plasma during glomerular
filtration
2) In the renal tubules the sodium ion reacts with carbonic acid formed from carbonic
anhydrous enzyme system
3) The bicarbonate anion form is reabsorbed and returns to the plasma and sodium ions reacts
with phosphate ion or lactate and excretion of phosphate ion takes place
4) The phosphate ion is also necessary for oxidation of alpha hydrides to generate high energy
products like ATP while the Co2 formed during metabolism is used in Krebs cycle.
5) There are other buffer system helps to remove the NH3 formed during metabolism of
proteins and amino acid.
The ammonia ion secreted by kidney tubules enters into tubular filtrate where it combines
with proton from carbonic acid to form ammonium ion.
IMPORTANCE OF ACID BASE BALANCE
The acid base balance in the body has to be maintained within the PH range 7.38-7.42
If the PH range is decreases below 7.38 so it will lead to acidosis.
If PH range is increased above 7.42, it will lead to alkalosis
Due to a variety of metabolic process in the body the acid level may be increased and the
alkaline level decreased below the normal range causing acidosis.
Acidosis occurs in conditions like congestive heart failure, pneumonia, Barbiturate and
narcotic poisoning.
The acid level may be decreased below the normal range and alkaline level increased from
the normal range causing alkalosis.
Alkalosis occurs in conditions like fever, Anoxia, salicylate poisoning.
The body restores the PH back to 7.38 7.42 by alteration in respiration and kidney function.
This condition is called compensated metabolic acidosis or alkalosis.
The body restores the acid base balance but the buffer ratio is still not brought back to normal
range. This is called uncompensated acidosis or uncompensated alkalosis.
Pharmaceutical Chemistry-I
86
Properties
White granular crystalline powder odourless having a bitter taste.
It is free dissolved in water and alcohol.
It efflorescence in warm dry air.
Addition of acid like Hcl, H2So4 form acetic acid.
Sodium acetate on treating with sulphuric acid and ethanol forms ethyl acetate which gives a
fruity odour
Identification test
Sodium acetate on treating with sulphuric acid and ethanol gives a fruity odour of ethyl acetate.
It reacts with ferric chloride it gives deep red colour.
Test for purity
It is tested for acidity, clarity and colour of solution , PH, arsenic, calcium, magnesium , heavy metals,
chloride, sulphate, reducing substances and lose on drying.
Pharmaceutical Chemistry-I
87
Properties
White crystalline odourless deliquescent in nature
Very soluble in water and alcohol
On strong ignition produces volatile non inflammable vapours and lives residue of potassium
carbonate.
It is alkaline to litmus.
Identification Test
The aqueous solution of potassium acetate gives the characteristic test for potassium and acetate.
Potassium acetate on treating with sulphuric acid and ethanol gives a fruity odour of ethyl acetate.
Test for purity
It is tested for Al, Ca, As, heavy metals, chloride, sulphate, acidity and alkalinity and lose on drying .
Test for aluminium and calcium: To aqueous solution of potassium acetate add dilute ammonia
solution and ammonium oxalate solution not turbidity or precipitate should be obtain
Lose on drying: Not more than 5% determined at 105oC .
Uses
It is used as a systemic alkaliser in condition like metabolic acidosis
Treatment of peptic ulcer
It is used as diuretic and urinary alkaliser
Pharmaceutical Chemistry-I
88
Properties
White crystalline odourless having a saline taste
Very soluble in boiling water and freely soluble in water and practically soluble in ether and
chloroform.
It is deliquescent in nature.
Heating at above 100C looses water molecule and on further strong heating it forms sodium
carbonate.
Presence of alcoholic hydroxyl group forms complex with blood constituents. Sodium citrate
forms complex with blood calcium to form an undissociated organic complex. Thus
producing anti coagulant action.
89
Storage
Stored in a well closed container. Protected from moisture since it is deliquescent in nature.
Sodium Lactate
Chemical formula:
Standard
It contains not less than 99% and not more than 101%
Preparations
By neutralising lactic acid with sodium carbonate or sodium hydroxide solution the solution is
filtered and evaporated to obtained crystals of sodium lactate.
Properties
Colourless odourless, amorphous powder
Soluble in water and insoluble in organic solvents
Contains asymmetric carbon atom and there are two stereo isomers namely D lactate and L
lactate.
The recemic mixture of lactate is present in injection forms
L lactate is converted sodium bicarbonate by metabolic oxidation inside the body.
Identification test
It is heated with potassium permanganate solution it gives acetaldehyde which is recognised
by its odour.
Test for purity
It is tested for acidity and alkalinity, clarity and colour of solution chloride, sulphate, calcium,
Magnesium arsenic, heavy metals and lose on drying.
Uses
It is used as fluid and electrolyte replenisher to maintain the acid base balance in the body.
It is used as systemic alkaliser since it is easily oxidised to give sodium bicarbonate.
Storage
Stored in a well closed container.
Electrolyte combination therapy
The electrolytes are combined in condition where there is excess loss of electrolyte from the body.
The electrolyte are lost the form of heavy lose of water, and electrolytes give to prolonged fever
severe vomiting, diarrhoea and cholera. These electrolytes can be administered in the form of
infusions and powders.
The electrolyte are combined and administered according to the need of the patient. There is a broad
section of commercially available infusion solution and powders which differed in the amount of
electrolytes. These combinations are divided into 2 main groups namely fluid maintenance and
electrolyte replacement.
Fluid Maintenance therapy is done with IV fluids which are intended to supply the normal
requirements of electrolytes to the patients who cannot take orally. All these solution contain 5%
dextrose. This therapy minimises the body built up of metabolites like urea, phosphates and ketone
body.
General electrolyte combination of maintenance solution contains 25 30 mEq/L of sodium, 1520mEq/L of potassium , 20-25mEQ/L of chloride and 20-23 mEq/L bicarbonate (or equivalent
amount of lactate or acetate ion) 3mEq/L of magnesium and phosphorous ion each.
Pharmaceutical Chemistry-I
90
There are two types maintenance solution: A solution for rapid initial replacement and a solution for
subsequent replacement of ions in the body for rapid initial replacement large concentration of ion
are required. It consists of 130 156 mEq/L of sodium ion, 4-12mEq/L of potassium and 98109mEq/L chloride ion, 28-55 mEq/L bicarbonate (or equivalent amount of acetate or lactate) 35mEq/L calcium and magnesium ions each.
The electrolyte concentration of subsequent replacement therapy consists of 42-121 mEq/L of
sodium, 16-35 mEq/L potassium, 30-103 mEq/L chloride, 16-53 mEq/L bicarbonate (or equivalent
amount of acetate or lactate), 5 mEq/L of calcium, 3-6 mEq/L of magnesium, 3 mEq/L of
phosphorous.
Eg: Infusions, injections compound sodium chloride solution or injection, powders (ORS).
ORS (Oral rehydration salt)
It is a combination of oral electrolytes. It is available in the form of powders and solutions.
They are required in conditions like a moderate to heavy lose of water and electrolyte.
Heavy loss of water and electrolyte occurs in conditions like severe vomiting, diarrhoea,
cholera and prolonged fever.
During these conditions there is marked depletion of lose of sodium ,potassium, bicarbonate
leading to metabolic acidosis.
To correct the dehydration and acidosis certain combination of essential electrolytes along
with sufficient amount of water has to be administered.
These preparations contain a typical concentration range of 130-160 mEq/L of sodium, 28-55
mEq/L of bicarbonate (or equivalent amount of acetate and lactate) 3-5 mEq/L of calcium, 3
mEq/L of magnesium along with glucose.
Glucose or dextrose present in this preparation helps to increase absorption of the electrolyte
and water in the small intestine.
ORS formula :
1) Sodium chloride 3.5gm
Potassium chloride 1.5 gm
Sodium bicarbonate 2.5gm
Glucose 20gm
Water 1Ltr
2) Sodium chloride 3.5gm
Potassium chloride 1.5 gm
Sodium citrate 2.9gm
Glucose 20gm
Water 1Ltr
Advantage
1) Very cheap than intravenous solution
2) No physician is required to administer it.
3) No need of sterilisation.
4) Patients can easily take the solution.
5) Vomiting is easily corrected by this therapy.
Administration
The powder is dissolved in boiled, cooled water and made up to 1ltr which is equivalent to 5
tumblerful.
Dosage
It depends upon the age and severity of dehydration. Infants and childrens require 1-2Ltr for a period
of 24hrs. Adults require 2-4 Ltr for a period of 24Hrs.
Model question Chapter wise
1. Explain the various officials preparations of sodium chloride.
(5)
Pharmaceutical Chemistry-I
91
Pharmaceutical Chemistry-I
92
e. Gases/Inhalants
These are drugs or chemicals which are in vapour form are inhaled or administered through the
respiratory system in body.
Medicinal Gases
Eg: Nitrous oxide, carbon oxide
Nitrous oxide
Chemical Formula: N2O
Synonym: Laughing gas, dinitrogen monoxide
Standard
Contain not less than 99% V/V of nitrous oxide.
Preparation
1. By chemical decomposition of ammonium nitrate nitrous oxide is obtained. The gas formed
purified by washing with sodium dichromate and sodium hydroxide solution. The purified gas
obtained is stored at compressed pressure in metallic cylinder at above 100 atm.
2. Heating mixture of sodium nitrate and ammonium sulphate nitrous oxide is obtained.
Properties
Colourless odourless weightless gas and dissolves in 2 volumes of water.
It gets liquefied at 50 atm pressure at 15oC.
It gets decomposed on heating at high temperature.
Identification Test
Pharmaceutical Chemistry-I
93
94
Identification Test
It is observed by alkaline pyrogallol solution.
The solution becomes brown. Mixed with equal volume of nitric oxide red fumes are produced.
Test for purity.
It is tested for acidity, alkalify carbon monoxide, carbon dioxide, hydrogen, oxidising substances,
tested for Co2.
Test for acidity/alkalinity; specified quantity of gas is passed through water containing specified
quantity of .1M HCl. Methyl red is added. No pink color is produced.
Test for CO2; by passing through Ba(OH)2, turbidity is not formed.
Test for oxidising substances: These are deducted by formation of blue colour by passing through a
solution of KI and starch solution.
For halogens: The gas is passed through a solution of AgNO3 no opalescence is produced.
Uses: It is necessary for normal respiratory function.
Used in the treatment of hypoxia in conditions like asthmatic attack shock, poisoning due to
gases.
Oxygen is mixed with 5-7% CO2 stimulate respiratory entre in brain.
Oxygen, helium mixture (2/:79) is used in treatment of patients severe lung diseases.
Inhalant to support respiration during anaesthesia.
Storage: Oxygen is stored in metallic cylinder under compressed pressure. The shoulder of
the cylinder is painted white and the remaining portion of the cylinder is painted black. The
symbol should be written on the shoulder.
Assay:
GASOMETRIC METHOD
The instruments used is nitro meter
Which is a specialised gas pipette and gas burette a certain volume of gas is drawn into the
gas burette it contain NH4cl and ammonium hydroxide Which is used as absorbing agent. the gas is
allowed to mix with absorption liquid. The volumes of unabsorbed gases such as nitrogen, hydrogen
are measured. The volume of residual gas is measured. The uncondensed gas should not exceed nmt
1v/v . It shows the presence of NLT 99% v/v of O2.
CO2
Standard: Contain not less than 99 v/v of CO2
Preparation: 1) Carbon is burnt with excess of oxygen carbon dioxide is obtained.
Pharmaceutical Chemistry-I
95
Calcium carbonate on reacting with Hcl, CO2 is obtained the gas is purified by passing
through K2CO3 and it is converted to K2HcO3 on heating at 100Oc it gives pure form of CO2.
Identification test:1. CO2 forms a precipitate of barium carbonate with a solution of barium hydroxide. The
precipitate dissolves with effervescence on addition of dilute acids like acetic acid.
2. Extinguishes a burning splinter.
Test for purity:
It is tested for acidity and alkalinity SO 2 gases organic reducing substance, hydrogen sulphate,
carbon monoxide.
SO2 is determent by colouration producing methyl orange and it is compared with a standard.
Phosphate & H2 and organic reducing substances are deducted by dark colouration when
through ammoniacal silver nitrate solution.
Uses: CO2 is used as respiratory stimulant.
A mixture of CO2 & oxygen is used to the treatment of carbon monoxide poisoning and for
treatment of poisoning drug like morphine.
Dry ice used for the treatment acne, psoriasis, warts, eczema by destroying tissues by freezing
it.
Storage
Pharmaceutical Chemistry-I
96
Stored in metallic cylinder under compressed pressure at cool temperature. Not exceeding
310c. The cylinder is painted gray having the symbol of CO2 on its shoulder.
Nitrogen:Standard: - It contain not less than 99% v/v of nitrogen
Preparation:1) Oxidation of ammonia with red hot copper oxide gives nitrogen.
By fractional distillation of liquid air the oxygen removed by passing through a solution of
sodium hydro sulphite or alkaline solution of pyrogalol, N2 is obtained.
Property: Colourless, tasteless odourless inert gas
Slightly lighter than air
Slightly soluble in water
It is liquefied to a colourless liquid
Boiling of 195.80c
Does not support combustion.
Nitrogen is a inert gas by reacts with oxygen in presence of high temperature to form nitro
oxide.
N2 reacts with H at reduced pressure of 200 900 atm pressure in the presence of catalyst
like Fe at 452oC form ammonia
N2 react with Mg to form magnesium nitride which on hydrolysis is give ammonia and
magnesium hydroxide.
Identification test: N will extinguish a burning splinter.
It is distinguished from CO2 by nitrogen will not turn lime water to milky.
Test for purity same CO2
Assay:Gasometric methods
N is assayed by gas metric methods. In this assay absorption agent is used is cuprous amino
chloride solution the gas is allow to mix with absorption liquid.
The volume of unabsorbed gases is measured the residual volume must not be less than 99%
v/v which corresponds to 99% of nitrogen.
Uses: N2 is an inert gas and it prevents oxidation.
It provides an inert atmospheric condition in containers containing ergometrine injection.
Vitamin preparations and fish liver oil
It is used for the manufacturing of ammonia and nitric acid.
Used as a diluents for pure oxygen
It is an important constituent present in amino acids, proteins.
Liquid nitrogen is used to freeze water.
Storage:
Stored in metallic containers under compressed pressure the cylinder is painted black and N2 symbol
is labelled on the cylinder.
Model question Chapter wise
1. Give the method & labelling of oxygen
(5)
2. Give the method & labelling of carbon dioxide
(5)
3. Give the method & labelling of Helium
(5)
4. Give the method & labelling of Nitrogen
(5)
5. Give the method & labelling of Nitrous oxide
(5)
Pharmaceutical Chemistry-I
97
Pharmaceutical Chemistry-I
98
Haemoglobi
n
Plasma
Haem
O2 transport
3g
%
of
body iron
65.4
Transferrin
Fe transport
4mg
.1
Functional
Iron
(Myoglobin)
Storage iron
Haem
Cellular
respiration
650mg
13.9%
1g
21.5%
Ferritin and Fe
pool
Haemosedri detoxificatio
n
n
4.65g
Pharmaceutical Chemistry-I
99
100%
Pharmaceutical Chemistry-I
100
Properties
Ferrous sulphate form green monoclinic crystals
It efflorescence in warm dry air
On exposure to moisture it undergo slow oxidation
Soluble in water and insoluble in alcohol
On heating Feso4 gets converted to ferric oxide
Identification Test
Feso4 or reaction with potassium Ferro cyanide forms a white ppt which gets oxidise on exposure to
air and gets darkened
FeSo4 reacts with solution of NaoH and NH4OH to form a green ppt
Test for purity
FeSo4 is tested for acidity and alkalinity, clarity and colour of solution, P H, As, Cu, Zn, Pb, Mn, heavy
metals, 5% solution of ferrous sulphate gives a PH between 3 and 4.
Assay
Oxidation reduction titration or redox titration
Pharmaceutical Chemistry-I
101
Weigh accurately about 1g of FeSo4 dissolved in 10ml of dilute H2So4 titrate against 0.1N KMnO4 .
The end point is appearance of pale permanent pink colour.
Uses
FeSo4 is used as haematinics
It helps in regeneration of Hb
Treatment of iron deficiency anaemia.
It used the preparation of FeSo4 tablets
Storage
Since it is effloresces in warm dry air and it oxidises in moist air. Stored in tightly closed containers.
Ferrous gluconate
CF:
Preparation
It is prepared from glucose. Glucose is oxidised by bacterial fermentation to give gluconic acid. It is
then treated with ferrous sulphate to give ferrous gluconate. It is crystallised with 2 molecules of
water of hydration and dried.
Properties
Yellowish gray or pale green, yellowish fine crystalline powder.
Soluble in water and almost insoluble in alcohol.
It has a slight odour of burn sugar
It is acidic in nature.
Identification test
Ferrous gluconate is dissolved in water and gives the characteristic test for ferrous iron and gluconic
acid. Gluconic acid is tested by dissolving in 7ml of water, 1 ml of glacial acetic acid and 1ml of
phenyl hydrazine. Heat it for 30 minute. Crystals of gluconic acid phenyl hydrazide is formed. The
crystals have melting point of 202.2oC.
Pharmaceutical Chemistry-I
102
Test for ferrous ion by reacting with a solution of potassium Ferro cyanide to form a white ppt which
gets oxidised on exposure to air and ppt gets darkened.
Test for purity
It is tested for acidity and alkalinity, As, Ba, ferric ion, Pb, chloride, oxalate, sulphate, dextrose
sucrose and loss on drying. Ferric ion is determined by iodometric method. Oxalate is determined by
precipitation as calcium oxalate. Dextrose and sucrose are determined by reduction of Fehling
solution after the removal of iron as ferrous sulphate.
Uses
It is used as haematinics
It helps regeneration of Hb
It uses the treatment of iron deficiency anaemia
Storage
Stored in light resistant containers since it is affected by light.
Ferrous Fumarate
Preparation
By double decomposition method, a hot aqueous solution of ferrous sulphate is added slowly to a
solution of sodium Fumarate with constant stirring, ferrous fumarate is obtained.
Properties
Reddish orange or reddish brown powder
Slightly having a characteristic odour
Astringent in taste
Slightly soluble in water and alcohol
Identification test
Ferrous iron reacts with potassium ferrocyanide to form a white ppt which gets darkened on exposure
to air.
Test for purity
It is tested for acidity and alkalinity, clarity and colour of solution. Chloride sulphate, As, Fe, ferric
salt and loss on drying.
Pharmaceutical Chemistry-I
103
Uses
It is used as haematinics
It helps in the regeneration of Hb
Treatment of iron deficiency anaemia
Storage
Stored in well closed light resistant container
IRON AND AMMONIUM CITRATE OR FERRIC AMMONIUM CITRATE
Fe(C6H5O7) x Fe(OH)3
Standard: Contains not less than 20.5% and not more than 22.5% iron. It is a colloidal solution of
ammonium ferric citrate.
Preparation
Ferric hydroxide is prepared by reacting sodium hydroxide and ferric sulphate. The ppt of ferric
hydroxide is collected and washed and the ferric hydroxide is removed by filtration. The syrup of
ferric hydroxide obtained is dried 40oc to obtain scales of ferric hydroxide. This ferric hydroxide is
reacted with citric acid to obtain ferric citrate. An excess of ammonia solution is added to obtain a
reddish brown scales of ferric ammonium citrate.
Properties
It is a complex of iron and ammonium citrate. It is present as reddish brown scales and
odourless.
It has astringent taste and deliquescent
Freely soluble in water and insoluble in alcohol
Identification test
Ignited gently and dissolve the residue in dilute Hcl. The solution gives the characteristic test
for ferric salts.
Warm the solution with NaoH and ammonia gas is evolved and the solution gives the
characteristic test for citrate.
Test for Purity
It is tested for the lead, As, chloride, free ferric compounds, sulphate and heavy metals. The free
ferric compounds are detected by adding to an aqueous solution of the substance potassium
ferrocyanide solution. No blue colour should be obtained.
Uses
It is used as haematinics
It helps the regeneration of Hb
This haematinics preparation is less irritating and less constipating compared with other
haematinic preparation.
Pharmaceutical Chemistry-I
104
Pharmaceutical Chemistry-I
105
Pharmaceutical Chemistry-I
106
Pharmaceutical Chemistry-I
107
Disorders
Mn deficiency leads to defective growth, bone abnormalities, reproductive dysfunction, CNS
dysfunction and improper fat and lipid metabolism.
The excess of Mn leads chronic magnesium or Manganase poisoning which has abnormal
body movement, mental disturbance and weakness of the body. It is treated by administering
levodopa.
Physiological Role of Molybdenum
It is a trace element present in the body
It is present as Co-Factors in enzymes like oxido reductases which is necessary for electron
transfer.
It is associated with Flavin depended enzymes
It is present in enzymes like xanthine oxidase sulphate oxidase and aldehyde dehydrogenase.
Requirements
Daily requirements are about 0.1 0.5mg for children. Daily requirements is 0.02-0.25mg
Therapeutic uses
The co precipitated complex of molybdenum oxide and ferrous sulphate is used as hematinic
Chromium
Physiological function of Cr
It is a trace element present in the body
It promotes glucose transport into the cell
It is a component of glucose, tolerance factor.
It helps in binding insulin to the cell membrane.
Disorders
Excess of Cr leads to nephritis, glycosuria, ulcers of skin and nasal mucosa
Requirements
Daily dietary requirement is 65-70 mcg.
Physiological function of Iodine
Iodine helps in thyroid hormone formation.
It helps in the synthesis of 2 thyroid hormones namely triiodiothyronine (T3) and thyroxine (T4)
Requirement
Daily requirement of iodine 140 mg for male 100 mg for female.
Disorders
Deficiency of iodine leads to enlargement of the gland called as simple or colloidal goitre.
The dietary deficiency of iodine causes endemic goitre. It is prevented by administering
iodised salt
Excess of iodine leads to irritation of skin, mucus membrane, conjunctivitis. This condition is
called iodism.
Therapeutic uses
Iodine is used for treatment of goitre and endemic goitre
It produces fibriolytic action and used in treatment of leprosy and syphilis.
It produces fungicidal action and uses in the treatment of fungal infections like
sporotrichosis, actionomycosis and blastomycosis.
Iodine in the form of KI used as expectorant
Official solution of Iodine
There are 3 types of official iodine solution
Pharmaceutical Chemistry-I
108
Pharmaceutical Chemistry-I
109
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
g. PHARMACEUTICAL AIDS
Pharmaceutical aids or excipients or diluents or inorganic agent used to increase the bulk of the active
ingredients and are used to convert the active drug in to an appropriate dosage form.
Ideal characteristic
It should be physically inert
It should be chemically inert.
It should not react with active drug.
It should not reduce the therapeutic activity of the active drug
Non-toxic
There are different types of excipients used in a dosage form like
1) Suspending agent
Eg: Bentonite, Sodium lauryl sulphate, sodium carboxy methyl cellulose
2) Lubricants
Eg: Magnesium stearate, talc, colloidal silica
3) Binding agents
eg: Starch, Polyvinyl pyrolidone
4) Preservatives or anti oxidants
eg: Sodium benzoate, sodium methyl paraben, sodiummeta bysulphite, sodium bysulphite
Pharmaceutical Chemistry-I
110
5) Coating agents
eg: Titanium dioxide
6) Vehicles or solvents
eg: Purified water, water for injection, sterile water for injection.
Suspending agents
These are inorganic agents which alter the surface characteristic of the solvent and reduces the
surface tension. They also acts as thickening agents.
They are widely used in preparation of suspension and emulsion.
Eg: Bentonite, sodium lauryl sulphate, sodium carboxy methyl cellulose
Bentonite
It is a native of colloidal hydrated aluminium silicate free from gritty particles.
Chemical formula
Al2o36Sio2.xh2o
Preparation
It is prepared from natural sources.
Properties
1) Very fine odourless cream coloured powder free from gritty particles
2) It has a slightly earthy taste and hygroscopic nature.
3) Insoluble in water and swells approximately 12 times of its volume to form a gel
4) It does not swell in organic solvent.
5) It is mostly composed of 90% mont morlinate and remaining 10% is feldspar.
6) It on decomposition shows the presence of aluminium silicate which is composed of silicon
dioxide , ferric oxide , aluminium oxide, calcium oxide, magnesium oxide and traces of
calcium , sodium and potassium.
7) Bentonite has particle size of 44 micron.
Identification test\
It dissolved in sodium carbonate solution and water and filtered. To the filtrate diluted Hcl
added which gives a gelatinous white precipitate.
Test for purity
It is tested for PH, heavy metals, sedimentation volume, swelling power, coarse particle and LOD.
Sedimentation volume
It is determined by mixing the sample with light magnesium oxide and suspend in water. The
suspension obtained is placed in a 100ml measuring cylinder. After 24Hrs the volume of clear
supernatant liquid is not more than 2ml.
Test for swelling power
The bentonite dissolved in small quantities at interval of 2minutes to solution of sodium lauryl
sulphate in a 100ml measuring cylinder. It is allowed to stand for 2Hrs . The apparent volume of
sediment at the bottom of the cylinder should not be less than 24ml.
PH A2% solution of bentonite gives a PH of 9 10.5.
LOD Not more than 15%
Uses
It is used in suspension and emulsion as suspending agent.
It is mainly used to suspend insoluble powders.
Stabilise emulsion
It is used as clarifying agent.
It used adsorbent for colouring substances.
It is used as an ingredient in the preparation of calamine lotion.
Pharmaceutical Chemistry-I
111
112
Preparation
It is prepared by reacting cellulose with sodium hydroxide in presence chloro acetic acid. Some of the
hydroxyl group present in cellulose are replaced by sodium acetate group (OCH 2COONa). The exact
number of acetate group entering the cellulose is variable. There are different grades of sodium
carboxy methyl cellulose are available.
Properties
Sodium carboxy methyl cellulose is a cellulose derivatives which is composed of large
number of Beta-D glucopyranose or glucose unit joint together by ether linkage.
There are about 2000-3000 glucopyranose unit corresponding to a molecular weight of about
3 lakhs 5lakhs are present.
When dissolved in water the solution has a viscosity of about 5-4000 centipoise.
It is a white or almost white granular powder odourless and hygroscopic in nature.
When dissolved in water it forms a colloidal solution.
It is practically insoluble in alcohol acetone, ether and toluene
Identification test
When dissolved in water at 40-60oC forms a colloidal solution to a portion of this solution Cuso 4
solution is added blue cotton like precipate is obtained.
The colloidal solution gives the characteristic test for sodium.
Test for purity
It is tested for PH, clarity and colour of solution apparent viscosity, chloride, sulphate, As, heavy
metals sulphated ash and LOD.
PH
The colloidal solution as a PH between 6&8
Clarity and colour of solution
The colloidal solution is a compared against a reference standard solution.
Apparant viscocity
It is determined by dissolving the substance in water at 90 oC. Dilute and stir the solution until a
complete solution is obtained. The viscosity of the solution is determined by using rotating
viscometer. The viscocity of this solution should be between 75&140%.
Sulphated ash
Between 20 and 33%
LOD
Determined at 105oC and should be below 10%.
Uses
It is used as suspending agent
It is used as thickening agent
It is used to increase the viscosity of liquid dosage form.
It is used as tablet excipient
It is used therapeutically as bulk laxative if taken internally.
Storage
Since it is highly hygroscopic should be stored in tightly closed container protected from moisture.
Magnesium stearate
Chemical formula: C`17H35100)2Mg
Standard
It contains varying proportion of Mg stearate along with Mg. Palmitate. It contains not less 3.8% and
not more than 5% of Mg.
Preparation
Pharmaceutical Chemistry-I
113
Calculated quantities of steric acid is added to a hot solution of NaoH constant stirring sodium
stearate is obtained on concentrating the solution. Then a solution of magnesium sulphate is added
and heated to obtain crystals of magnesium stearate. Finally washed and dried.
Properties
White, unctuous powder and non toxic in nature.
It is decomposed by mineral acids like Hcl to form stearic acid.
Identification test
Mg stearate is decomposed by nitric acid. The fatty acid (stearic acid) is extracted by ether. The fatty
acid after removal from ether should melt at not less than 52 oC. The filtrate gives a characteristic test
for Mg.\
Test for purity
It is tested for acidity and alkalinity, chloride, sulphate, As, Pb, heavy metals, free fatty acid, acid
value, Zinc, stearate and LOD
Acid value
Should between 195-210
Test for free fatty acid
The free stearic acid is determines by dissolving the substance in chloroform filter evaporate. The
solution on a water bath the residue obtained is dissolved in ethanol and titrated agains 0.1M NaoH
using phenolphthalein ad indicator.
Uses
It is used as a lubricant in tablet manufacturing.
It is used as a suspending agent.
It is used as baby dusting powder.
Preservative
These are substances used in small conc in pharmaceutical dosage from to prevent the microbial
growth.
The preservatives prevent the spoilage of dosage form.
It provides stability to a dosage from like tablet and capsules.
Eg: Benzoic acid (0.1%) antibacterial preservative in liquid dosage form.
Sodium benzoate (0.1%) Antifungal preservative.
The above 2 preservatives are used in liquid dosage form like a suspension, emulsion and
solutions.
Methyl paraben sodium Antibacterial preservative
It prevents microbial growth in tablets and capsules.
Sodium benzoate
Standard
It contains not less than 99% and not more than 101% of sodium benzoate.
Chemical formula
C6H5COONa
Pharmaceutical Chemistry-I
114
Preparation
Sodium carbonate is added to a hot conc. Solution benzoic acid until the liquid is just alkaline to
litmus. The salt obtained is evaporated to obtain crystals of sodium benzoate.
Properties
White crystalline powder hygroscopic, odourless to faint odour of benzoin and saline taste.
It gets hydrolysed by mineral acids like Hcl to form benzoic acid.
Identification test
To aqueous solution of sodium benzoate in diluted Hcl gives white precipitate the characteristic test
for benzoic acid and sodium.
Test for purity
It is tested for acidity and alkalinity, As, Pb, chloride, sulphate, chlorinated compounds and loss on
drying.
Test for chlorinated compounds;
Dissolve in Na2CO3 solution. Evaporate to dryness. Heat below 400C until it gets charred. It gets
converted to NaCl and extracted with dil HNO3 and filtered. To the filtrate perform the limit test for
chloride.
Uses
It is used as antifungal preservative
It is used as preservative in liquid dosage form like suspension and emulsion
Food preservative.
Storage
Stored in a well closed container protected from moisture.
Sodium methyl paraben
Standard
Pharmaceutical Chemistry-I
115
It contains not less than 99% and not more than 102% of sodium methyl paraben calculated with
reference to dried substance.
Preparation
Sodium methyl paraben is prepared from 4-hydroxy benzoic acid which is prepared from heating a
solution of potassium salicylate and diluted Hcl. 4-hydroxy benzoic acid is esterified with methanol
in presence of conc. H2So4. The methyl ester obtained (Methyl paraben) is dissolved in sodium
hydroxide solution to obtain sodium methyl paraben.
Properties
White crystalline odourless an hygroscopic powder.
Freely soluble in water and sparingly soluble in ethanol.
Identification Test
The substances dissolved in water and acidified with concentrated Hcl. The infrared spectrum
of the methyl paraben should be concordant with spectrum obtained from standard methyl
paraben.
The solution obtained from the previous test gives the characteristic test for sodium.
Test for Purity
It is tested for acidity and alkalinity, clarity and colour of solution, P H, chloride, sulphate, Fe, As,
heavy metals and LOD.
PH
0.1% of the substance should have a PH between 9.5 to 10.5
LOD
Not more than 5%
Uses
It is used as antibacterial preservative
It is used as a preservative particularly in solid dosage form like tablets and capsules.
It is primarily used as preservative against yeast.
It is more effective when used in combination with propyl paraben sodium in the ratio of 2:1
Storage
Stored in a well closed container and protected from moisture.
Antioxidants
Antioxidants are reducing substances added to a drug or a pharmaceutical dosage form to prevent
their oxidation through various oxidative processes.
The are used in pharmaceutical preparation containing easily oxidisable substances in order to
maintain these substances in their original form.
Mechanism of antioxidant action
The mechanism of antioxidant action involves
Pharmaceutical Chemistry-I
116
Properties
White crystalline powder with pungent irritating odour.
Freely soluble in water slightly soluble in alcohol.
It reacts with acid to form sulphurous acid
It is powerful reducing agent and reduces iodine, permanganate, dichromate, halogens ferric
salt, hydrogen peroxide and gets oxidise to form sodium bisulphate
Pharmaceutical Chemistry-I
117
Identification Test
A solution of sodium bisulphite reacts with Hcl and turns a filter paper moistened with
mercurous nitrate to black
A aqueous solution gives the characteristic test for sodium
Test for Purity
It is tested for acidity and alkalinity, chloride, sulphate, As, Fe, Sulphite, heavy metals, LOD.
Uses
It is used as anti oxidant preservative (0.1-0.2%).
It is used as antiseptic.
0.2% solution of sodium bisulphite is used as an anti oxidant to preserve adrenalin phenyl
ephedrine hydrochloride and ascorbic acid injection.
It is used as reducing agent for solubilising dyes and permanganate as stain remover.
It is uses externally for parasitic skin diseases.
It is used as stabilising agent
Storage
Stored in a well closed container protected from moisture and light.
Sodium metabisulphite
Chemical Formula
Na2S2O5
Synonym
Disodium pyrosulphite, sodium pyrosulphite
Standard
It contains no less than 95% and not more than 100.5%
Preparation
Sodium metabisulphite is prepared by passing So2 gas into a hot concentrated solution of NaoH until
it gets saturated. Sodium bisulphite is Ist formed which is unstable and gets converted to sodium
metubislphite. The solid sodium meta bisulphite separates as a crystal on cooling.
Properties
Colourless white crystalline or creamy white powder with sulphurus odour and saline taste.
Freely soluble in water, slightly soluble in alcohol.
It is a powerful reducing agent and reduces iodine, permanganate and ferric salt.
Pharmaceutical Chemistry-I
118
It form sodium bisulphite formed reacts with acids like diluted hcl to form sulphurous acid
which is unstable and liberate sulphur dioxide gas.
Test for Fe
Fe present gets oxidise to ferric salt by reacting with a solution of bromine and NH 4thio cyanate. The
solution produces a red colour which should not be darken than producer by a standard solution of Fe
similarly treated.
Test for thisulphate
Dissolve 1g of the substance in 10ml of diluted Hcl heat on a water bath for 10 minutes and should
not produce a pale opalescence.
Uses
Antioxidant preservative
It is used as antioxidant and stabilizes injections of adrenalin and morphine.
It is a powerful reducing agent and used to prepare water soluble derivatives of insoluble
drugs.
It is used as preservative for acidic solution and syrups.
It is used as antioxidant for substance which are readily oxidise to coloured decomposition
products.
Storage
Stored in a tightly closed light resistant container in a dry place.
Sulphur dioxide
Chemical Formula
So2
Standard
Contains not less than 97 % v/v of So2 gas
Preparation
Pharmaceutical Chemistry-I
119
Properties
Colourless gas non inflammable with pungent irritating odour.
Soluble in water.
The aqueous solution is acidic to litmus
So2 forms addition product with halogens
under the influence of oxygen and heated forms SO3
It act as a reducing agent and reduces iodine to iodide ions permanganate to magnese salt and
iodates to iodine
Identification Test
1) The filter paper moistened with potassium iodide and starch solution and dried. It is exposed
to sulphur dioxide gas and develops a blue colour on continuous exposure to So 2 the blue
colour disappears.
2) The filter paper moistened with mercuric nitrate is exposed to So 2 gas , it becomes black due
to the reduction of mercuric nitrate to mercury.
Test for Purity
It is tested for acidity and alkalinity, chloride, sulphate, sulphide impurities, Cu, Fe, As and heavy
metals.
Uses
It is used as antioxidant preservative
Pharmaceutical Chemistry-I
120
2. Large scale preparation: By heating kaolin or china clay in boiling H2So4 solution aluminium
sulphate is obtained.
Properties
White crystalline powder, odourless having a sweet astringent taste.
Soluble in cold water and freely soluble in hot water and practically insoluble in alcohol.
It efflorescence to varying degree of water of crystallisation.
2% solution of aluminium sulphate is acidic an in nature
Aqueous solution of aluminium sulphate has a PH of 3
It forms double salt with sulphates or alkali metals which is known as alum
On heating aluminium sulphate looses water of crystallisation and on strong heating it gets
decomposes to form alumina and sulphur trioxide gas.
121
Pharmaceutical Chemistry-I
122
By adding to purified water diluted Hcl and BaCl2. The appearance of the solution should not change
atleast for 1 hour. If sulphate is present turbidity will be produced.
Test for oxidisable substances
It is detected by adding acidified KMnO 4 and boil the solution the solution should remain faint pink
is produced if oxidisable susbstances are present the solution gets decolourise.
Test for residue on evaporation
It is performed to detect the presence of no volatile matter. Evaporate the purified water in water bath
and it is dried to a constant weight at 105oC. The residue obtained should not be more than 0.001%
Uses
It is used as pharmaceutical aid.
It is used as solvent for the preparation of liquid Dosage form.
It is used in the preparation of several official preparations of solution tinctures and extracts.
It is used in the preparation of various test reagents.
Water for injection
It is distilled water free from pyrogens.
Preparation
It is prepared by demineralisation or by ion exchange treatment of purified water and passing this
solution through metallic still or distillation unit.
The purified water is distilled using metallic still and filtered with and efficient device such as baffles
to prevent the entrapment of droplets. The distilled water obtained by this method is free from
pyrogens. The solution obtained is not sterilized.
Test for Purity
It is tested for pyrogen bacterial endotoxin, P H. It is also tested for Cu, Fe, Chloride, sulphate, NH 3,
oxidisable substances non volatile matter and albuminoid matter.
PH 4.5-7.5
Refer purified water.
Uses
Used a solvent preparing parental preparation.\
It is used for manufacturing of ophthalmic preparation.
It is used a solvent for the preparation of various injection preparation.
Storage
Stored below 4oc or above 31oc.
Sterile water for injection
It is sterilized water for injection and suitably packed.
Preparation
Water for injection is sterilized by autoclave and other sterilisation method to obtain sterile water for
injection.
Properties
Clear colourless and odourless liquid.
It should not contain any antimicrobial substances.
It should be free from pyrogens.
Test for Purity
It should be tested for acidity and alkalinity, NH 3, Ca, Mg, heavy metals, chloride, sulphate, nitrate,
copper, Fe, oxidisable substance . It should comply the test for sterility and pyrogens.
PH
4.5 7.5
Pharmaceutical Chemistry-I
123
Higher limits of oxidisable substances and non volatile matter are permitted because of
slightly gain in these substance during sterilisation.
Uses
It is used as a solvent in the preparation of parenteral preparation prepared by aseptic process.
It is also used as a solvent for ophthalmic preparation prepared by aseptic process.
It is also used as a solvent for the preparation of injections of aqueous solution or suspension.
Storage Stored in a single dose container preferably in type 1 or type 2 glasses.
Model question Chapter wise
1. Explain the following terms with example
(5)
(i) Preservatives
(ii) Anti-oxidant
(iii) Suspending agent
2. Give the ideal properties of anti-oxidants with example
(5)
3. Write briefly about suspending agents
(5)
4. Write briefly about solvent & vehicles
(5)
5. Write the various pharmaceutical aids in formulation
(5)
6. Write the preparation & uses of sodium bi sulphite
(5)
7. Write the preparation & uses of sodium meta bi sulphite
(5)
8. Write the preparation & uses of magnesium stearate
(5)
9. Write the preparation & uses of sodium benzoate
(5)
10. Give the requirements for water for injection
(5)
11. Explain the difference between purified water & water for injection
(5)
12. Write the preparation, assay & uses of sodium bi sulphite
(5)
13. Write the preparation, assay & uses of sodium meta bi sulphite
(5)
14. Write the preparation, assay & uses of sulphur dioxide
(5)
15. Write the preparation, assay & uses of bentonite
(5)
16. Write the preparation, assay & uses of magnesium stearate
(5)
17. Write the preparation, assay & uses of aluminium sulphate
(5)
18. Write the preparation, assay & uses of sodium benzoate
(5)
19. Write the preparation, assay & uses of sodium CMC
(5)
20. Write the preparation, assay & uses of sodium methyl paraben
(5)
21. Write the preparation, assay & uses of sodium lauryl sulphate
(5)
22. Write the preparation, assay & uses of purified water
(5)
23. Write the preparation, assay & uses of water for injection
(5)
24. Write the preparation, assay & uses of sterile water for injection
(5)
H. Miscellaneous agents
ANTIDOTES
These are inorganic agent which counteract or neutralises the action of poisons. The poison is the
substance which endangers life by affecting one or more vital function
Mechanism of antidote
These are three type of mechanism in which antidote acts.
1) Physiological antidote
These antidote acts by producing a change in the physiological response of a poison. The
produce opposite effect in the physiology and there by neutralises the action of poison.
Eg: Sodium nitrite (NaNO2). It is used in cyanide poisoning . sodium nitrite oxidises Fe2+ ion
of haemoglobin to Fe3+(Meth haemoglobin). This meth haemoglobin bind cyanide to form
cynomethhaemoglobin which is non toxic.
Pharmaceutical Chemistry-I
124
2) Chemical antidote:
These antidote produce a change in chemical nature of the poison. The toxic poisons
converted into non toxic form by chemical reaction.
Eg: Sodium thiosulphate
3) Mechanical antidote
It acts by adsorbing the poison in the body and there by prevent the toxic effect of poison.
Eg: Activated charcoal, it adsorbs poison before the poison is adsorbed across the intestinal
wall.
Sodium Nitrite
Chemical form: NaNo2
Standard: Contains not less than 98% , not more than 101% of sodium nitrate calculated with
reference to dried substance
Preparation
By strongly heating sodium nitrate, sodium nitrite is obtained.
Heating sodium nitrate with metallic led and reducing at law temperature, sodium nitrite is
formed the product is dissolved in water, the solution is filtered , the insoluble led acid is
removed, the product is evaporated to obtain the crystals of sodium nitrite.
By absorbing nitric oxide gas into a solution of sodium carbonate and catalytic oxidation
produce sodium nitrite
Properties
White crystalline powder having a saline taste
Freely soluble in water
Sparingly soluble in alcohol
On exposure to atmospheric air it slowly oxidised to sodium nitrate.
Easily decomposed by acidification with diluted H2So4 and finally converted to NO2 gas
Pharmaceutical Chemistry-I
125
It reduces KI to iodine
Oxidise KmnO4 to manganese sulphate.
Identification test
The aqueous solution of NaNO2 gives characteristic test for sodium nitrite.
Test for purity
It is tested for chloride, sulphate, iron, As, cyanide, acidity, alkalinity, led and lose on drying.
Uses
Used as antidote for cyanide poisoning
Used as antioxidant
Prevents the growth of clostridium botulinum spores in preparation
Used in meat packing to maintain the deisired red colour.
Dose: it administered in IV form of 10-15ml of 5% sodium nitrite solution.
Storage
Stored in a well closed container. Protected from moisture and light, since it gets converted into
nitrate form.
Sodium thiosulphate
Chemical formula: Na2S2O3 5H2O
Standard: Contain not less than 98% not more than 101% Na2S2O3.
Preparation: To a solution of Na2CO3, sulphur dioxide gases passed resulting in the formation of
sodium bisulphite. It on further reaction with Na 2CO3 forms sodium sulphite. Finally on treatment
with sulphur results in the formation Na2S2O3
By passing SO2 gas into a solution of solution sodium suphide. Sodium thosulphate is formed.
Properties
Colourless, crystalline powder
Pharmaceutical Chemistry-I
126
Identification test
To an aqueous soln of substance addAgNO3, a white ppt is produced and becomes quickly yellowish
and finally becomes a black ppt.
To aq soln, I2 soln is added the colour gets discharged.
Test for purity
It is tested for the presence of arsenic, calcium, heavy metals, P H, sulphite, sulphate, clarity and
colour of solution and loss on drying.
Pharmaceutical Chemistry-I
127
Test for sulphate: Tested for these impurities. It is obtained during the manufacturing by oxidation of
compound with iodine solution and applying the limit for sulphate.
Sulphite is limited by adding aqueous solution of freshly prepared sodium nitroprusside. The solution
should not become violet.
Uses
Chemical antidote.
Used as antidote in cyanide poisoning along with sodium nitrite.
It is used to convert toxic cyanide to non toxic thiocyanide.
Used as antioxidant
Widely used in iodometry and iodimetric titration
Storage
Stored in a well closed container, protected from moisture.
ACTIVATED CHARCOAL
Ref under adsorbents and protectives
Uses
Used as antidote for treatment of aspirin paracetamol and chloroquine poisoning
mechanical antidote.
Used for the preparation of universal antidote
Sedatives
These are inorganic agent, that produce mild depressions of CNS and reduce excitements and calms a
patient.
Eg: KBr
It produces sedative
Potassium Bromide
Chemical formula: KBr
Standard: Contain not less than 99% and not more than 101% fk Br. Calculated with reference to
dried substance.
Preparation
1) Prepared by adding excess of bromine to the solution of KOH potassium bromate and KBr is
formed. Potassium bromate is reduced by charcoal.
Pharmaceutical Chemistry-I
128
Standard
Ammonium carbonate contains varying proportion of ammonium bicarbonate and ammonium
carbomate that yields between 40-45% ammonia.
Preparation
By subliming a mixture of ammonium sulphate or ammonium chloride with CaCo 3 in iron retorts and
condensing the vapours in chambers, lined with lead ammonia along with ammonium carbonate is
recovered by passing, into H2So4 solution
Properties
White hard, crystalline powder, freely soluble in water.
The strong odour of ammonia
It is volatile at above 60oC and it gives ammonia vapours.
Partially soluble in alcohols and the residue of ammonium bicarbonate is found at the bottom
of the alcoholic solution conforming the partial solubility.
Pharmaceutical Chemistry-I
129
Aqueous solution of the salt is alkaline when it exposed to air. It partially dissociates and
volatilises and converted into white powder.
Readily soluble in water and NH3 soln to form normal ammonium carbonate.
When it exposed to air it loses ammonia and Co2 and gets converted to hard translucent
substance.
It decomposed by the addition of mineral acid. The acid may be added to a dry salt or to a
solution of salt in water.
Identification Test
To a little of the salt is heated. It is volatilise and no charring take place. When tested with moist
litmus paper vapours are strongly alkaline.
Uses
Used as respiratory stimulant,
Used as a source of ammonia used in the preparation of aromatic NH3 spirit.
Aromatic ammonia spirit contain ammonium carbonate and strong ammonia solution
Storage
Stored in a cool place, air tight container, protected from light.
Selerosing agents
There are irritating agent used to damage the wall of a vein resulting in its occlusion. It is used for the
treatment of varicose vein and haemorrhoids.
Eg: sodium tetra decyl sulphate
Sodium tetra decyl sulphate
Standard
It contains concentration of 46-52% of sodium dodecyl so4
Preparation
It is prepared by sulphating tetra dodecyl alcohol and converting into its sodium salt.
Properties
White waxy, odourless solid.
Soluble in water, alcohol, ether.
Identification Test
The aqueous solution of gel adds Methylene blue solution. Diluted H 2So4 , chloroform and shake well
chloroform layer becomes intensely blue.
The substance gets hydrolysed, hot ethanol solution with diluted Hcl and filtered. The filtrate barium
chloride solution is added. White crystalline precipitate is obtained.
Test for Purity
Tested for alkalinity, non esterified alcohol, chloride, sulphate, sulphated ash,
Pharmaceutical Chemistry-I
130
Test for non esterified alcohol: non esterified alcohol are long chain fatty alchol which are
unsulphated and remain in the sample in aqueous solution. Extract repeatedly with n-pentane.
The extract is dried with anhydrous Na2SO4. Filtered and evaporated in a water bath at
105oC and weighed.
Uses:
Used as sclerosing agent and treatment of haemorrhoids
Treatment of varicose vein
Hypertonic saline or Sodium chloride hypertonic injection
Standard
It is a saline preparation containing 1.6% W/V of sodium chloride in water for injection contains 270
mmol/L of sodium and chloride ions/Ltr
Properties
Clear colourless solution aqueous solution as pH between 5-7.5
Identification Test
The aqueous solution gives a characteristic test for sodium and chloride ions.
Test for Purity
It is tested for chloride, sulphate, heavy metals and bacterial endotoxin. The bacterial endotoxin not
more than .5 endotoxin unit/ml
Uses
It used as sclerosing agent for treatment of varicose vein.
Treatment of haemorrhoid.
It used as fluid and electrolyte replenisher in case of severe electrolyte imbalance.
Storage
Stored in a single dose container made up of glass or plastic all keeping small solid particles may
separate to the top of the container.
And such injection containing visible solid particles should not be used.
EXPECTORANT (Mucokinetics)
These are inorganic agents used to orally to enhance the secretion of sputum by air passages. So that
it easy to remove the phlegm through coughing. These agents facilitate the flow of respiratory tract
secretion which will allow the ciliary motion by inducing of coughing to move the loosen material
towards the pharynx more easily.
They are used in respiratory disorders in which the secretions are excessive and viscous in nature.
This agent increases the bronchial secretion or making it less viscous.
The are widely used in various cough preparation.
Classification
These agents are classified based on the mechanism of a action.
1. Direct Action
These agents act directly on the bronchial secretory cells and there by stimulate the flow of
respiratory tract secretion.
Eg: Terpene hydrate.
2 Indirect action
These agents act indirectly by irritating the gastric mucosa thereby acting on the bronchial
secretory cells and there by stimulate the flow of respiratory tract secretion.
Eg : KI, NH4Cl
Potassium iodide
Pharmaceutical Chemistry-I
131
Chemical formula
:
KI
Standard
:
Not less than 99% not more than 101%
Preparation
By action of iodine on potassium hydroxide
By heating a hot aqueous KOH with iodine a mixture of KI and KIO 3 are formed . The potassium
iodate formed is reduced by activated charcoal to form potassium iodide.
Properties
Large transparent, colourless or white crystalline odourless, saline and slightly bitter taste.
Stable in dry air.
Deliquescent in moist air.
Very soluble in water, glycerine and alcoholic glycerine
Aqueous solution of KI takes of iodine. When iodine is dissolved them and form poly iodide
(KI3) which is equilibrium with dissolved iodine.
Test for purity
By adding to an aqueous solution of KI, a definite volume of 0.01M sulphuric acid using
phenolphthalein as indicator no colour changes is produced.
Test for Burium
By adding dilute H2SO4 to an aqueous solution of KI, no turbidity is produced.
Test for Cynide
To an aqueous solution ferrous sulphate solution and add NaOH solution and acidified with diluted
Hcl no blue colour is produced.
Test for Iodate
To an aqueous solution add dilute H2SO4 and starch solution no blue colour is produced. Iodate react
with KI and liberate iodine will give blue colour with starch .
Uses
Used as an expectorant
Used as a source of iodine
Used as prophylaxis and treatment of goitre.
Treatment of thyrotoxicosis.
Mild antifungal agent.
Preparation of iodised salt
Storage
Store in air tight containers protected from light since it is deliquescent slightly in moisture
Model question Chapter wise
1. Explain briefly sclerosing agents
2. Write about note on sedatives
3. Name one compound with chemical formula from each class
(a) Respiratory stimulant
(b) Sedatives (c) Expectorant
4. Give the preparation & uses of hypertonic
5. Give the preparation & uses of sodium tetradecyl sulphate
6. Give the preparation & uses of ammonium chloride
Pharmaceutical Chemistry-I
132
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(5)
(10)
(10)
(10)
(10)
(10)
(10)
(10)
(10)
Co-ordination compounds
Pharmaceutical Chemistry-I
133
The maximum number bond formed by the ligand with the metal ion is called co-ordination
number
Theory of co-ordination compounds: It is explained by Werners theory
Werner studied the complex formation
The order of stability of ligand in the complex formation depends upon the basicity.
The ligands can be classified with various types based on number of position of molecules
capable of co-ordinating with metal ions.
Unidentate ligand
These ligands have one non bonded pair of electrons to donate to the metal ion to form one
co-ordinate covalent bond in complex formation.
Bidenlate ligand
There ligands have two co-ordinate number and both acts as donor to the metal ion.
134
Pharmaceutical Chemistry-I
135
Therapeutic uses:
It is a drug of choice for arsenic metal poisoning
It is used the treatment of mercury poisoning.
It is used as antidote for metal poisoning like lead, gold and copper poisoning
It is a contraindicated poisoning due to iron, selenium and cadmium.
Penicillamine
Chemical structure
Chemical name , dimethyl cysteine
Properties
Penicillamine is the degradation product of penicillin.
White crystalline powder having a slight characteristics odour.
Freely soluble water, slightly soluble in alcohol.
Aqueous solution as a pH 4.5 to 5.5.
Antidote mechanism
Penicillamine is used as antidote for copper poisoning. It forms soluble complex with copper and it
will reduce Cu2 + ions in tissue to Cu1+ ions in sulphhydral groups of enzyme. Cu1+ is complexed
tetrahedrally to form dipenicillamine Cu1+ complex. This complex is water soluble and hence easily
excreted from the body. Thus reducing the increased concentration of copper ions in the blood.
Structure
EDTA
It is availably two salt forms namely disodium EDTA and calcium disodium EDTA.
Disodium EDTA
Chemical structure
Chemical formula
Synonym disodium edetate
Pharmaceutical Chemistry-I
136
Properties:1, 10 Phenanthroline is a complexing agent which forms stable highly coloured complex with
a metal in two different oxidation states. Hence 1,10 Phenanthroline metal complex is used as an
indicator in oxidation- reduction titration.
It forms complex with copper, iron, zinc and other metals.
The complex formed by 1,10 Phenanthroline with ferrous ion is called ferroin indicator. This
indicator is used in assay involving Cerric ammonium sulphate.
Structure
Pharmaceutical Chemistry-I
137
Uses: It is used in redox titration where cerric ammonium sulphate is used as oxidizing agent
Eg:- It is used the assay of ascorbic acid tablets and ferrous gluconate tablets.
Model question Chapter wise
1. Write the stability of co-ordination compounds.
(5)
2. Explain the following terms
(5)
(i) Ligand
(ii) Co-ordination member
(iii) Sequestering agent
3. Write a note on Ligands.
(5)
4. Give the treatment for arsenic poisoning
(5)
5. Give the treatment for copper poisoning
(5)
6. Give the treatment for Heavy metal poisoning
(5)
7. Explain the application of co-ordination compounds.
(5)
8. Explain theory of werners.
(5)
9. Give the application of EDTA & Dimercaprol
(5)
10. Give the application of penicillamine & 1,10 phenanthroine.
(5)
11. Explain in detail the application of co-ordination compounds.
(10)
12. Give the structure mechanism of action & therapeutic uses of EDTA & penicillamine. (10)
13. Give the structure mechanism of dimer caprol & 1,10 phenanthroine.
(10)
Complete the equations
GIT
Acidifier
1. Nacl+H2SO4
2. NaHSO4+Nacl
3. NH3+Hcl
4. NaOH+Hcl
5. Na+Hcl
6. Na2CO3+Hcl
7. NaHCO3+Hcl
8. AgNO3+Hcl
9. Na2SO3+Hcl
10. Na2S+Hcl
11. Na2S2O3+Hcl
12. Na2CO3+H3PO4
13. Ca3(PO4)2+2H2 SO4
14. Ca(H2PO4)2+Na2CO3
15. Na2HPO4 on heating
16. Na2HPO4+Nacl2
17. Na2HPO4+Frcl3
18. Na2HPO4+Pl(CH3COO)2
19. (NH4)2MoO4+Na2HPO4+HNO3
20. NH3+Hcl
21. AgNO3+NH4cl
22. AgNO3+NH4SCN
23. NH4cl+HCHO
Pharmaceutical Chemistry-I
138
1. Na2CO3+CO2+H2O
NaHCO3 on heating
2.
3. NaHCO3+Hcl
4. K3C6H5O7+O2+O2
5. KHCO3+H3C6H3O7H2O
6. Na2CO3+KAl(SO4)2+H2O
7. Al(OH)3+HCl
8. AlCl3 H2O+Na2HPO4
9. MgO+H2O
10. MgSO4+NaOH
11. Mg(OH)2+H2SO4
12. MgSO4+Na2CO3+H2O
13. MgCO3 Mg(OH)2 H2O+HCl
14. MgCO3+Disodium EDTA
15. Mg2Sl3O8+HCl
16. Ca(OH)2+CO2
17. CaCl2+Na2CO3
18. CaCO3+CO2+H2O
19. CaCO3+NH4Cl
20. CaCO3+HCl
21. Bi(NO3)3+Na2CO3+H2O
22. Bi+HNO3
23. {(Bi O)2CO3)}2 H2O on heating
24. BiCl3+H2O
25. BiCl3+H2S
26. Mg O+H2SO4
Topical agents
1. Zn+O2
2. ZnCO3-Zn (OH)2
3. ZnO+HCl
4. ZnO+NH4OH
5. C17H35 COONa+ZnSO4
6. (C17H35COO)2 Zn+HCl
7. FeTiO3+HCl+Cl2
8. Al2(SO4)3+K2SO4
9. ZnO+HCl
10. Zn+H2SO4
11. BaO2+H2SO4
12. BaO2+H3PO4
13. Na2O2+H2SO4
14. H2O2 on heating
15. KMnO4+H2SO4+H2O2
16. KOH+MnO2+KclO3
17. K2MnO4+Cl2
18. KMnO4+H2SO4
19. KMnO4+H2O
20. H2C2O4. H2O+KMnO4+H2SO4
Pharmaceutical Chemistry-I
139
Dental products
1.
2.
3.
4.
5.
6.
7.
8.
HF+Na2CO3
CaF2+Na2CO3
NaF+ HCl
NaF+H2O
FeCl3+NaF
SrO+HCl
Sr(OH)2+HCl
SrCO3+HCl
Gases
1. NaHCO3 on heating
2. Na2CO3+H2SO4
3. CO2+H2O
4. NaOH+H2CO3
5. Ca(OH)2+CO2
6. CaCO3+H2O+CO2
7. CO3+C on heating
8. NH4NO3 on heating
9. NaNO3+(NH4)2SO4
10. N2O
11. C+N2O
12. S+N2O
13. Cu+N2O
Pharmaceutical Chemistry-I
140
14. NH3+CuO
15. N2+O2
16. N2+3H2
17. Mg+N2
18. Mg3N2+H2O
Pharmaceutical aids
1.
2.
3.
4.
5.
6.
7.
Na2CO3+H2SO3
NaHSO3+HCl
NaHSO3+I2+H2O
NaHSO3+Na2CO3
NaHSO3 on heating
NaOH+SO2
Na2S2O3 on heating
Pharmaceutical Chemistry-I
141
8. I2+Na2S2O5+H2O
9. Na2S2O3+HCl
10. S+O2
11. FeS2+O2
12. H2SO4+Cu
13. Cu2S+O2
14. SO2+O
15. I2+H2O+SO2
16. SO2+Cl2
17. KIO3+H2O+SO2
18. KMnO4+H2O+SO2
19. C17H35COONa+MgSO4
20. (C17H35COO)2 Mg+HCl
21. Al2O3+H2SO4
22. Al2(SO4)3H2O
23. Al2(SO4)3 on heating
24. 2C6H5COOH+Na2CO3
25. C6H5COONa+HCl
26. C6H5COONa+NaOH
27. C6H5COONa+H2SO4
28. C6H5COONa+FlCl3
Miscellaneous
1. Kl3
2. KOH+I2
3. KIO3
4. KOH+BI2
5. NaBCO3+C
6. KMnO3+KBa+H2SO4
7. NaNO3+C+Ca(OH)2
8. NaNO3+Pl
9. NaNO3+NaOH+S
10. NaNO2+H2SO4
11. HNO2+KI+H2SO4
12. NaNO2+KMnO4+H2SO4
13. Na2CO3+NaHSO3
14. Na2SO3+S
15. Na2S2O3 on heating
16. Na2S2O3+HCl
17. Na2S2O3+AgNO3
18. Na2S2O3+I2
19. Na2S2O3+BaCl2
20. (NH4)2 SO4+CaCO3
21. Amonium carbonate on heating
22. Amonium carbonate +HCl
Pharmaceutical Chemistry-I
142
Pharmaceutical Chemistry-I
143
Pharmaceutical Chemistry-I
144
Pharmaceutical Chemistry-I
145
Pharmaceutical Chemistry-I
146
Pharmaceutical Chemistry-I
147
Pharmaceutical Chemistry-I
148
Pharmaceutical Chemistry-I
149
Pharmaceutical Chemistry-I
150
Pharmaceutical Chemistry-I
151
Pharmaceutical Chemistry-I
152
Pharmaceutical Chemistry-I
153
Pharmaceutical Chemistry-I
154
Pharmaceutical Chemistry-I
155
Pharmaceutical Chemistry-I
156
Pharmaceutical Chemistry-I
157
Pharmaceutical Chemistry-I
158
Pharmaceutical Chemistry-I
159
Pharmaceutical Chemistry-I
160
Pharmaceutical Chemistry-I
161
Pharmaceutical Chemistry-I
162