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PROCESS VALIDATION PROTOCOL


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PAGE NO:- 1 0F 25

FORMULATION

PRODUCT NAME :
LINE

REASON FOR PERFORMING THE VALIDATION STUDY :


Reason ( tick which ever is applicable)

Remarks

Department
New product
Modification in the manufacturing process.
Change in Facility and / or location of manufacturing.
Batch fail to meet product & process specifications.
Number of batches studied: ________________
Batch numbers:
1. _______________
2.. _______________
3. _______________
Validation activity authorized By: _____________________________Date:_______________________
Validation Team:
DEPARTMENT

VALIDATION TEAM

PRODUCTION
QUALITY ASSURANCE
QUALITY CONTROL
REMARKS:
APPROVALS:
DEPARTMENT

SIGN & DATE

PRODUCTION
QUALITY ASSUARANCE
QUALITY CONTROL
PRODUCT DEVLOPMENT
ENGINEERING

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1.0 GENERAL:
1.1 INTRODUCTION:
The process validation will be performed as prospective validation . The complete documentation for
the validation comprises several independent documents, references to relevant documents will be given
as part of this protocol, (see below). The results of the validation activities will be summarized in the
validation report.
1.2 LIST OF DOCUMENTS FOR VALIDATION:
Validation protocol,
Details of sampling for the validation batches, test parameters ( Product performance characteristics)
with reference to test methods & Acceptance criteria. (acceptable Limit)
Methods for recording / evaluating results including statistical analysis.
Reference to relevant documents.
1.2.2 BATCH MANUFACTURING RECORDS.
Detailed manufacturing instructions for the production of the validation batches.
2.0 PERSSONEL RESPONSIBILITIES.
SR
1
2
3
4

ACTIVITY
Preparation of validation protocol
Approval of Validation protocol
Production of validation Batches
Testing of validation samples &

Preparation of validation report


Approval of validation report.

RESPONSIBILITY

REMARKS

3.0 PROCESS DESCIRPTION / FLOW SHEET

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The information given below provides a general description of the process. Detailed information for the
manufacturing will be supplied separately in the batch manufacturing record.
1.0 DISPENSING OF MATERIAL
2.0 WATER PHASE PREPARATION
3.0 OIL PHASE PREPARATION
4.0 MIXING
5.0 Q.C APPROVAL
6.0 FILLING , CRIMPING & CODING.
7.0 PACKING
3.1 FORMULATION:
BATCH SIZE:
SR

Ingredients/excipients

Specification

Label
claim

Per
batch

Qnty of
overages

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
NOTE:

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3.2 FLOW SHEET:


DISPENSING OF MATERIAL

ADDITIONAL QUALITY OF
WATER ADDED.
TEMP.
SPEED( RPM)
MIXING TIME

WATER PHASE
PURIFIED WATER

HEAT

OIL PHASE
____ MINS./ SLOW

____ MINS./ SLOW

Addition Of
Excipient

1. MIXING TIME
2. SPEED( RPM)
3. TEMP.

Addition Of
Active
Ingredient

Mixing
With Addition Of Active
Ingredient
____ Mins./ Slow

1. MIXING TIME
2. SPEED( RPM)
3. TEMP.

Q.C APPROVAL
WEIGHT / TUBE
CRIPING
CODING

FILLING , CRIPING &


CODING

FINAL PACKING

4.0 EQUIPMENT / FACTORY.

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A detailed list of equipment used for validation together with the cleaning status will be provided in
the manufacturing documents.
4.1 LIST OF SOPS , VALIDATION & QUALIFICATION REPORT USED AS REFERENCES
SR

ID. NUMBER

1.

TITLE

VERIFIED
BY

Equipment cleaning procedure for Octagonal Steam


Jacketed Tank 350 ltr with stirrer ( for Oily Phase)
Equipment Operating procedure for Octagonal Steam
Jacketed Tank 350 ltr with stirrer ( for Oily Phase)
Equipment operating procedure for 500 ltr.
manufacturing tank with Homonizer and anchor stirrer.
Equipment cleaning procedure for 500 ltr manufacturing
tank with Homonizer and anchor stirrer.
Equipment cleaning procedure for storage tank.
Equipment operating procedure for storage tank
Equipment cleaning procedure for Tube filling machine
Equipment operating procedure for Tube filling machine
Enter any other reference sop.

2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.

4.2 DETAILS OF EQUIPMENT TO BE USED.


EQUIPMENT
BALANCE

DETAILS
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TYPE :
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WATER PHASE
S.S.TANK

OIL PHASE TANK :

MFG. TANK :

EQUIPMENT
STORAGE TANK:

TUBE FILLING
MACHINE:

TRANSFER PUMP:

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PAGE NO:- 6 0F 25

MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.

DETAILS
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.
TYPE :
MODEL:
CAPACITY:
MANUACTURER:
TAG.NO.:
M.O.C.

REMARKS:
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4.3 IDENTIFICATION OF CRITICAL PROCESS VARIABLES/ PARAMETER.


4.3.1 PROBABLE CAUSES THAT MAY EFFECT FINAL PRODUCT:
DISPENSING OF
MATERIAL

OIL PHASE SOLUTION


PREPARATION

TUBE FILLING

LOAD SIZE

SPEED

ACTIVE

SPEED

WEIGHT/TUBE

TEMPERATURE
EXCIPIENT

PH

TEMPERATURE

COOLING
TEMPERATURE

SPEED

SPEED

LOAD SIZE
BOILING
TEMPERATURE
Prepared by
WATER PHASE
SOLUTION
PREPARATION

LOAD SIZE

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CRITICAL PROCESS PARAMETERS:


SR
1

CRITICAL PRECESS
VERIABLE
WATER PHASE SOLUTION
PREPARATION
Sequence of excipient addition
Water Boiling Temperature
Time
Heating Temperature
Time
Cooling Temperature
Time
PH
Mixing time
OIL PHASE SOLUTION
PREPARATION
Sequence of excipient addition
Heating Temperature
Time
Cooling Temperature
Time
Mixing time
MANUFACTURING
Sequence of Active addition
Mixing time
Cooling Temperature
Filling, Crimping & Coding
Filling speed

RESPONSE PARAMETER

REMARKS

Water phase uniformity

Fixed order of addition


Fixed Boiling temperature range
Variation of time for boiling
Fixed Heating temperature range
Variation of time for heating
Fixed cooling temperature range
Variation of time for cooling
Fixed limit of Ph
Variation of mixing time (RPM)

Oil phase uniformity


Fixed order of addition
Fixed Heating temperature range
Variation of time for heating
Fixed cooling temperature range
Variation of time for cooling
Variation of mixing time (RPM)
Active ingredient uniformity

1. Weight of tube
2. Crimping

Fixed order of addition


Variation of mixing time
Fixed temperature range
Fixed machine speed, no
variation.

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CRITICAL PROCESS VARIABLE:


SR

PROCESS / VARIABLE

MACHINE SETTING

Water Phase Solution

(CONTROL VARIABLES)
Quantity of water

Preparation
Oil Phase Solution

Quantity of paraffin & wax

Preparation
Manufacturing

& other oil.


Mixing time

Filling

Cooling Time
Speed, weight / tube.

REMARKS

Setting and conditions as mentioned in


the batch manufacturing record to be
followed.

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5.0 SAMPLING , TEST PARAMETERS, ACCEPTANCE CIRTERIA


5.1 Sampling Locations:
Mfg. Tank.

1. TOP SAMPLE A1

2. MIDDLE SAMPLE A2

3. BOTTAM SAMPLE A3
BOTTOM VALVE

5.3 SAMPLING
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STAGE/ TEST PARAMETER


Water phase solution preparation

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SAMPLING
( SIZE,LOCATION,TIME)
After the completion of water

Record amount of water ,

phase solution ,

Temperature & time required to

N=1 sample ( pooled from

achieve desired end point/ ampere

different locations)
Oil phase solution preparation

PH,
ASSAY

Filling

reading.

Sample size =20 gm


After the completion of Oil phase

Record amount of oil,

solution ,

Temperature & time required to

N=1 sample ( pooled from

achieve desired end point/ ampere

different locations)
MANUFACTURING

REMARKS

Sample size =20 gm


After 20 min of mixing time,
After 30 minutes & after 40
minutes.
N=3 samples at each interval
Sample size: 20 gm
Draw the sample entire filling

reading.
Record the pH and assay of active
content .

Each sample comprises the

assembly, consisting of transfer

amount for the different tests

pump & holding tank and filling

required.

Identification test

machine.

Appearance

Sample draw from each

Uniformity of Weight

syringes as a set weight at

Assay of active content.

different time interval.


Sampling : at start, every two
hours, immediately after the
brake time , end of filling..
Sample size :__________.

STAGE / TEST PARAMETER

EQUIPMENT
( SIZE , LOCATION, TIME)

ACCEPTANCE CRITERIA

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Water phase solution preparation


Oil phase solution preparation
Manufacturing

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PAGE NO:- 12 0F 25

Determination on each sample, for

80 + 50C

temperature, sample weight 10 g.


Determination on each sample, for
temperature, sample weight 10 g.
Sampling thief:

80 + 50C

ASSAY

Assay 90 % to 110 %
Rel. std. :

PH

FILLING
Appearance

Visual inspection,

As specified in the BMR.

Weight of Tubes.

Analytical balance

_____ gm (_____gm - _____ gm)

Weight variation

Analytical balance

_______ % of average weight.

Identification test

H.P.L.C.

Test should complies to its


specifications.

90 % to 110 %
Assay:

6.0 RECORDING OF DATA & DATA TREATMENT

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6.1DATA RECORDING
The data obtained from the various analysis & observations shall be recorded in the DATA
RECORDING SHEET for first three commercial batches.
DATA RECORDING
SHEET NO.
SHEET NO 1
SHEET NO 2
SHEET NO 3
SHEET NO 4
SHEET NO 5
SHEET NO 6
SHEET NO 7
SHEET NO 8
SHEET NO 9
SHEET NO 10

For recording water phase mixing observation & results


For recording oil phase mixing observations & results.
For recording Bulk manufacturing observations & results.
For recording assay results after filling and crimping operation.
For recording general utilities /equipment / method Analytical /results.
For recording analytical method validation.

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DATA RECORDING SHEET #1


WATER PHASE SOLUTION PREPARATION
Equipment Name

:_________________________

Identification no

:_________________________

Capacity

: ______________________lt.

Date:___________________

Ingredients and sequence of material addition: ____________________


Total weight of ingredients

: _______________kg/lot.

Mixing time

: 20 minutes

Setting stirrer

: slow

Procedure

: As outlined in the batch manufacturing record.

Plan

: Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing

from 3 different locations


FOR WATER PHASE SOLUTION TANK-RESULTS.

BATCH NO:

Assay of after mixing AT 20 MIN..


Sample no:
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL

Temperature

RESULTES
Uniformity

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Assay of after mixing AT 30 MIN..


RESULTES
Sample no: Temperature
Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Assay of after mixing AT 40 MIN..
RESULTES
Sample no: Temperature
Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
Actual Temperature of the water/binder : ___________ 0C
Temperature of the water after heating : ___________ 0C
Temperature of the water after cooling : ___________ 0C
Additional quantity of water added (ltr.):____________
Total time taken
: ___________
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria.
YES (
)
NO (
)
CONCLUSIONS:________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
__
CHECKED BY:_________________________

DATE____________________
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DATA RECORDING SHEET # 2


OIL PHASE SOLUTION PREPARATION
Equipment Name

:_________________________

Identification no

:_________________________

Capacity

: ______________________lt.

Date:___________________

Ingredients and sequence of material addition: ____________________


Total weight of ingredients

: _______________kg/lot.

Mixing time

: 20 minutes

Setting stirrer

: slow

Procedure

: As outlined in the batch manufacturing record.

Plan
from 3 different locations

: Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing

FOR OIL PHASE SOLUTION TANK-RESULTS.


Assay of after mixing AT 20 MIN..
Sample no:
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL

Temperature

BATCH NO:

RESULTES
Uniformity

Assay of after mixing AT 30 MIN..


RESULTES
Sample no: Temperature
Uniformity
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL
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Assay of after mixing AT 40 MIN..


Sample no:
1
2
3
Average std.
Dev.
Range
RSD
LCL
UCL

Temperature

RESULTES
Uniformity

Actual Temperature of the water/binder : ___________0C


Temperature of the water after heating : ___________0C
Temperature of the water after cooling : ___________0C
Additional quantity of water added (ltr.):____________
Total time taken

: ___________

POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria.
YES (
)
NO (
)
CONCLUSIONS:________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
__

CHECKED BY:_________________________

DATE____________________

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DATA RECORDING SHEET # 3


MANUFACTURING :
Equipment Name

:_________________________

Identification no

:_________________________

Capacity

: ______________________lt.

Date:___________________

Ingredients and sequence of material addition: ____________________


Total weight of ingredients

: _______________kg/lot.

Mixing time

: 20 minutes

Setting stirrer

: slow

Procedure

: As outlined in the batch manufacturing record.

Plan

: Samples to be drawn at of 20 minutes, 30 minutes, & 40 minutes of mixing

from 3 different locations


FOR MANUFCTURING TANK-RESULTS.
Assay of after mixing AT 20 MIN..
Sample no:
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL

PH

Assay of after mixing AT 30 MIN..


Sample no:
PH
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL

BATCH NO:

ASSAY

REMARK

ASSAY

REMARK

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Assay of after mixing AT 40 MIN..


Sample no:
1
2
3
Average std. Dev.
Range
RSD
LCL
UCL

PH

ASSAY

REMARK

POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria.

YES (

NO (

CONCLUSIONS:________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
__

CHECKED BY:_________________________

DATE____________________

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DATA RECORDING SHEET # 4


FILLING & CRIMPING :
Equipment Name

:_________________________

Identification no

:_________________________

Capacity

: ______________________lt.

Date:___________________

Mixing time( filling hopper) : Continues stirring during filling


Setting stirrer

: slow ( R.P.M._________)

Procedure

: As outlined in the batch manufacturing record.

Plan

: Samples to be drawn from each syringes as set weight at different time


interval as mention below:

1. Initional ( 0 time)
2. Every 2 hours
3. Immediately after the break time
4. At the end of filling
from 3 different locations
FOR FILLING MACHINE -RESULTS.
SAMPLE NO:

APPEARANCE

BATCH NO:
WEIGHT IDENTIFICATION ASSAY
TEST

Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling
Average std. Dev.
Range
RSD
LCL
UCL

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Assay of after mixing AT 30 MIN..


SAMPLE NO:
Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling

APPEARANCE

WEIGHT IDENTIFICATION TEST

ASSAY

WEIGHT IDENTIFICATION TEST

ASSAY

Average std. Dev.


Range
RSD
LCL
UCL
Assay of after mixing AT 40 MIN..
SAMPLE NO:
Initional ( 0 time)
Every 2 hours
Immediately after the
break time
At the end of filling

APPEARANCE

Average std. Dev.


Range
RSD
LCL
UCL
POINTS
Method of analysis adopted
Ref No.:
Analyst:
Date
Meet acceptance criteria.

YES (

NO (

CONCLUSIONS:________________________________________________________________________
______________________________________________________________________________________
______________________________________________________________________________________
__
CHECKED BY:_________________________

DATE____________________
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DATA RECORDING SHEET # 5


DATE:____________________
SR

NAME OF CRITICAL EQUIPMENT/UTILITIES

1
2

S.S 350 Octagonal Steam Jacketed Tank.


S.S 350 Octagonal Steam Jacketed Tank.

3
4
6

( OIL PHASE)
500 Octagonal Steam Jacketed Tank
Storage Vessel
Filling ,crimping & Coding machine

QUALIFICATION/
VALIDATION FILE
REF.NO.

DATE OF
QUALIFICATION /
VALIDATION

UTILITIES:
1
AHU SYSTEM
2
WATER SYSTEM
3
COMPRESSED AIR
4
STEAM
5
LIGHTNING
6
DRAIN

DATA RECORDING SHEET # 6


DATE:____________________
NAME OF PRODUCT:
SR Parameters

Type of
sample

Sample A
(known
amount of
analysis.

Accuracy
% Recovery of
known amount.

Actual
reading

Observed
reading

Analysis
performed
by

Analysis
checked by

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sheet

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90 % of A
110 % of A
Precision
Sample A1
Repeatability
( from one
( under same
sample
condition ) Test point)
by same analyst Sample A2
at same time
( from
from same
second
homogenous
sample
validated mass
point)
but from
Sample A3
different sample ( from third
plan ( by taking sample
sample of
point)
different
quantity)
Reproducibility Sample A1
under different
On ______
conditions.
Sample A2
On ______
Test by
different analyst Sample A3
on different
On ______
days.

SR Parameters

Type of
sample

25 % of A
50 % of A
75 % of A
100 % of A
125 % of A

Linearity and range


Response
concentration curve
on graph paper.

Actual
reading

Observed
reading

Analysis
Analysis
performed checked
by
by

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sheet

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Specificity/
selectivity( by
larger
communication of
analytical method.)
for identification of
impurities assay of
active component
etcTemp &
humidity /
degradation
factored to main
ingredients by 15
min, 30 min,45 min
of heating or
known degraded
products.
Limit of detection
( LOD) & limit of
quantitative (LOQ)
Qualitative &
Quantitative result

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PAGE NO:- 24 0F 25

Sample A1
15 min.
degradation

Sample A2
30 min.
degradation

Sample A3
45 min.
degradation
0.1 % of A
1% of A
5 % of A
10 % of A

Analysis method
(for non
pharmacopoeial to
be performed by
other public lab.

20 % of A
Method A
Method B
Method C

REMARKS:
1. Specifically / selectivity analysis(4) and Reproducibility (2B) also given raggedness and robustness.
2. Limit of Quantitative (5) also gives sensitivity of test procedure.
Above procedure to be repeated over three batches to get minimum nine variables for each parameter.
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