Professional Documents
Culture Documents
1
I CNG
Mc tiu hc tp
Trnh by nh ngha thuc v cc yu cu BCL
thuc
Trnh by h thng t chc, qun l, kim tra cht
lng thuc ti Vit Nam
Trnh by ni dung cng tc tiu chun ha
Trnh by cc ni dung chnh ca KTCL thuc:
-Ly mu
-Kim nghim
-Vit phiu & tr li kt qu
Ni dung chnh ca GLP
Cht lng thuc v m bo cht lng
Khi nim v thuc
WHO
iu l thuc phng bnh, cha
bnh (24/1/1991)
nh ngha chnh thc
v thuc ti Vit Nam
Ngun gc: ng vt, thc vt, khong
vt, sinh hc
i tng s dng: con ngi
Mc ch s dng:
- Phng, cha bnh
- Phc hi, iu chnh chc nng
- Lm gim triu chng
- Chn on
- Phc hi, nng cao sc khe
- Lm mt cm gic mt b phn hay ton thn
- Lm nh hng qu trnh sinh sn
- Lm thay i hnh dng c th
- Vt liu nha khoa, bng bng, ch khu y t
THUC
Cht lng thuc v m bo cht lng
Cht lng thuc
Tng hp cc tnh cht c trng ca thuc (nh
tnh, nh lng, tinh khit, nhn, bao gi)
Th hin mc ph hp vi yu cu k thut
nh trc ty theo iu kin kinh t, k thut,
x hi
m bo t cc mc ch:
- C hiu lc
- Khng hoc t tc dng c hi
- n nh v cht lng trong thi hn xc nh
- Tin dng, d bo qun
Cht lng thuc v m bo cht lng
Yu cu cht lng thuc
- ng thnh phn theo t l quy nh ca cng thc
ng k v c cp php (nh tnh, nh lng)
- c php SX v SX ng quy trnh ng k
v c cp php
- Tinh khit t quy nh
- ng gi trong ng, bao gi vi nhn
thch hp, ng quy cch ng k
- c bo qun, phn phi, qun l ng quy
nh CL thuc c duy tr trong sut tui th
ng k hay thi hn bo hnh
Cc yu t m bo cht lng (cc GP)
Nguyn liu
Thnh phm
Sn xut
Bo qun
Phn phi
GLP
GSP
GDP
GPP
GMP
GACP
Yu t lin quan mt thit n kim nghim thuc
2/23/2014
2
Thc hnh tt sn xut thuc (GMP)
Cc quy nh cht ch, chi tit v mi mt
qu trnh sn xut sn xut thuc:
- Thnh phn theo d kin
- t tiu chun k thut t ra
Yu cu
- Quy trnh sn xut
- Con ngi
- C s vt cht
- Kim tra, theo di trong qu trnh sn xut
- H thng h s sn xut, phn phi
- C ch thu hi sn phm
Thc hnh tt phng KN thuc (GLP)
Cc quy nh cht ch, chi tit v mi mt
qu trnh KTCL thuc:
- m bo kq chnh xc, khch quan.
Yu cu
- Con ngi
- C s vt cht
- Ha cht, thuc th, cht chun
- iu kin v sinh
- Ly mu, lu mu
- Th nghim, x l s liu
- Lu tr h s
Thc hnh tt bo qun thuc (GSP)
Cc quy nh cht ch, chi tit v mi mt
qu trnh tn tr, iu kin bo qun, xut
nhp nguyn ph liu, bao b, thnh phm,
nhn m bo CL thuc n ngi sd.
Yu cu
- Con ngi
- C s vt cht
- iu kin v sinh
- Quy trnh bo qun, vn chuyn
Thc hnh tt nui trng, thu hi DL (GACP)
Yu cu
- Nhn dng, xc nh ngun gc cy thuc
- Ging, vt liu nhn ging
- Trng trt, thu hi, ch bin, tn tr
- Con ngi
- C s h tng, trang thit b
- H s, ti liu
Cc quy nh trong nui trng, thu hi dc
liu c ngun nguyn liu tho dc cht
lng tt, an ton mt cch bn vng, bo
tn ngun dc liu v mi trng.
Kim tra cht lng thuc
Mc tiu
- Ngi s dng dng c thuc m bo cht
lng, t hiu qu s dng cao
- Pht hin thuc khng t tiu chun, thuc gi,
thuc km phm cht x l
Quy nh
Tt c thuc v NL lm thuc u phi c KN
v xc nh cht lng, nu t tiu chun quy
nh mi c a vo s dng
Kim tra cht lng thuc
Khi nim:
KTCL thuc (KN thuc) l vic s dng cc pp phn
tch xc nhn mt thuc hay nguyn liu t hay
khng t tiu chun quy nh.
- C phi l thuc cn kim tra khng?
- C m bo hot lc, hm lng ng k khng?
- C t tinh khit yu cu khng?
- C b bin cht, phn hy khng?
- bao gi, nhn c ng quy cch khng?
2/23/2014
3
Kim tra cht lng thuc
Yu t nh hng
- Ri ro, nhm ln, khng chp hnh quy nh
GMP
- Sn phm c hm lng thp hn quy nh do
v tnh hay c trong SX
- Cng thc, k thut bo ch cha ng lm
thuc b phn hy, bin cht
- Qu trnh bo qun cha tt
- Thuc gi
Thuc t, khng t tiu chun
Thuc t tiu chun
p ng y cc yu cu KT ca TC
ra (hay p ng y cc mc cht lng
trong TCCL ng k)
Thuc khng t tiu chun
p ng khng y cc yu cu KT
ca TC ra hay ng k (c th khng
t mt hay nhiu ch tiu). Thuc khng t
TC thuc loi thuc km cht lng.
Thuc gi, thuc km phm cht
Thuc gi
- Khng c hot cht hoc hm
lng khng m bo
- Cha dc cht khc vi trn
nhn
- Nhi kiu dng cng nghip
Thuc gi, thuc km phm cht
Thuc km phm cht
Khng t tiu chun trc
t v nhiu nguyn nhn khc
nhau:
- Sn xut, bo qun
- Nguyn liu, bao b
- Qu hn SD
- Mi trng
Trung ng a phng
- Vin KNTTW
- Vin KNT Tp.HCM
Cc TTKN thuc, m phm
tnh, thnh ph
H thng KTCL
H THNG QUN L, KIM TRA CHT LNG THUC
Doanh nghip,
CSSX
Phng Kim nghim, KCS
Phng nghip v Dc
B Y t
S Y t cc tnh, thnh ph
Cc Qun l Dc
H thng QLCL thuc
Cc QLD
Xy dng quy hoch, ln k hoch v QLCL thuc,
t chc thc hin k hoch c ph duyt
Xy dng vn bn php quy v TC& CL thuc
BYT ban hnh, hng dn, kim tra vic thc hin
Qun l ng k TCCS. Cung cp TT v BCL thuc
Ch o, gim st h thng KTCL thuc trn ton
quc
Kim tra, cp giy chng nhn GMP, GLP
T chc hng dn nghip v cho CBQLCL, o
to bi dng nghip v v TC- L- CL thuc
Phi hp thanh tra BYT thc hin chc nng
kim tra, thanh tra NN v CL thuc, x l vi phm
2/23/2014
4
H thng QLCL thuc
Ph bin, hng dn, t chc thc hin cc vn
bn PL v QLCL thuc ti a phng.
Thc hin chc nng kim tra, thanh tra NN v CL
thuc, x l vi phm v CL thuc trong phm vi
a phng
Phng
Nghip v
Dc
S y t
H thng KTCL thuc
Nghin cu xy dng TCVN v thuc (DVN).
Kim tra, xc nh CL thuc trn th trng
Vin KNT
Tp.HCM
Vin KNT
TW
Thm tra KT, gip BYT xt duyt TCKN cp
ng k SX v lu hnh thuc ti VN
Pht hnh cht chun, cht i chiu cho KN
Lm trng ti v CL khi c tranh chp khiu ni v CL
thuc
Tham gia o to CB lm cng tc KN
T vn v chnh sch CL thuc QG
Xy dng TC PKN t GLP, gip , kim tra cng
nhn GLP trong c nc
Kim tra vic KN thuc theo TC trong c nc
H thng KTCL thuc
Nhim v gii hn trong phm vi tnh, thnh ph
TTKN
tnh,
thnh ph
H thng
t KTCL
ca c s
Xy dng TCCS cho cc sn phm do c s SX
Kim tra nguyn liu, bao b, bn thnh phm,
thnh phm
Cng tc tiu chun ho
Tiu chun ha:
Mt lnh vc hot ng gm 2 ni dung
Xy dng ra cc tiu chun
p dng TC trong thc t
Mc tiu
a hot ng XH (SX, KD) vo n np
t hiu qu chung c li nht cho mi
ngi & XH
Cng tc tiu chun ho
Tiu chun:
Nhng quy nh thng nht v hp l
c trnh by di dng vn bn hoc th
thc nht nh
Do mt c quan c thm quyn ban hnh
Bt buc p dng cho nhng ni c lin quan
TC
Vn bn php ch
Quy nh thng nht, hp l
Bt buc p dng nhm BCL mt s/p
Cng tc tiu chun ho
Cht lng sn phm:
Mt tp hp nhng ch tiu c trng
Th hin tnh nng s dng
Nhm tha mn yu cu xc nh trc
cho sn phm trong nhng iu kin xc
nh
Ph hp vi hon cnh kinh t, k thut, XH
2/23/2014
5
Cng tc tiu chun ho
Tiu chun thuc:
Vn bn KHKT mang tnh php ch quy nh
Quy cch
Ch tiu yu cu KT
Phng php th
ng gi- ghi nhn- bo qun
Cc vn lin quan khc
Cng tc tiu chun ho
Tiu chun thuc:
L c s c s KN
Tin hnh thc nghim
nh gi kt qu
Cng b kt qu (Phiu KN)
nh gi CL thuc t hay khng t, c
c php lu hnh khng
Tiu chun thuc
Edwin Smith Papyrus
(Ai Cp)
Dc in Vit Nam IV (2010)
1500 T.C.N
1617 : London Pharmacopoeia
1864 : British Pharmacopoeia
1820 : USP
1971: DVN I
2010: DVN IV
Lch s
Cng tc tiu chun ho
i tng
-Thit b, dng c, my mc
-Sn phm, hng ha
-Nguyn vt liu
-Nguyn tc, th tc, phng php
-Thut ng, o lng, k hiu
Tiu chun thuc
L mt TC ton din, gm nhiu ni dung
Th hin mc CL thuc c to ra v duy tr
cho ti khi s dng hoc ht tui th
NI DUNG CHNH
1.Tiu
2.Yu cu k thut
3.Phng php th
4.ng gi, ghi nhn, bo qun
Ni dung chnh ca tiu chun thuc
1
Tiu
Tn nguyn liu, thnh phm
Tn n v ban hnh TC
Loi TC
Hiu lc thi hnh
2/23/2014
6
Ni dung chnh ca tiu chun thuc
2 Yu cu k thut
ra mc CL hp l ca sn phm
(mi YCKT l 1 ch tiu hay tiu ch)
L c s cho vic:
-Lp k hoch SX
-Thc hin k hoch (s lng, CL)
-Qun l (kinh t, k thut, gi, k kt
hp ng, khiu ni)
Ni dung chnh ca tiu chun thuc
3 Phng php th
M t chi tit quy trnh th nghim,
quy trnh phn tch xc nh xem
mt ch tiu c t YCKT t ra
hay khng
Ni dung chnh ca tiu chun thuc
4 ng gi, ghi nhn, bo qun
Mi thuc lu hnh phi c nhn n n v
ng gi nh nht
Nhn phi c ni dung cn thit gip nhn
bit:
-Thuc
-Cch s dng
-Tn CSSX, SK, SKS, HD, iu kin bo qun
Phi c quy nh r
Tiu chun thuc
Cp tiu chun
Tiu chun Dc in Vit Nam (TCVN
v thuc)
Tiu chun c s:
-TCCS ca sn phm lu hnh trn th trng:
phi ng k vi CQ c thm quyn. Cc mc TC
khng c thp hn quy nh trong DVN
-TCCS ca thuc pha ch trong n v (khng
lu hnh trn th trng) do th trng V xt
duyt, ban hnh.
TCVN v thuc:
- NN y quyn cho BYT bin son, xt
duyt, ban hnh sau khi ng k ti Tng
cc LCLNNVN
- Cc TCVN v thuc c tp hp li thnh
Dc in VN
TCCS:
Do CSSX bin son, c cp c thm
quyn duyt
Cng tc xy dng tiu chun Cng tc xy dng tiu chun
Th tc xy dng tiu chun
Chun b ti liu, kho st thc t, lp cng
XD d tho TC ln 1:
- Tham kho TL
- xut cc ch tiu, phng php th
- Kho st thc t v SX, s dng sn phm
- SX th, lm thc nghim phn tch cc TC d
kin
- Vit d tho TC v thuyt minh
- Lp d tho bin php p dng
- Thng qua d tho ti c s
2/23/2014
7
Cng tc xy dng tiu chun
Th tc xy dng tiu chun
Hon thnh d tho TC sau khi ly kin gp
sa cha, hon chnh h s gi CQ qun l xt
duyt
Xt duyt v ban hnh TC:
-CQ qun l cp TC no th xt duyt, ban hnh
TC .
-Trc khi xt duyt, TC phi c gi qua CQ
thm tra k thut (VKN, TTKN) v c quan php
ch (Cc QLD, phng nghip v Dc)
-Th trng BYT hoc GSYT k duyt sau khi
tham kho CQ thm tra.
Cng tc xy dng tiu chun
Th tc xy dng tiu chun
H s TC gm tt c:
- Vn bn KHKT
- Kho st NC
- Cng vn trnh duyt
- Quyt nh xt duyt
Cng tc xy dng tiu chun
Phng php xy dng yu cu k thut
Cc ch tiu ca YCKT:
- Cng dng: tinh khit, hm lng
- Tin cy, an ton: hn dng, bn
- Tm sinh l: dng bo ch, ng dng
- Thm m: ng gi, bo qun
Cng tc xy dng tiu chun
Phng php xy dng yu cu k thut
Ni dung chnh ca YCKT:
- Cng thc pha ch: phi trnh by cng thc
pha ch ca thuc, ghi r tn nguyn ph liu, s
lng (bng s, bng ch), TC nguyn ph liu
- Cht lng thnh phm: Nu r hnh thc, t/c
cm quan (hnh dng, th cht, mu sc, mi v),
cc im c bit, yu cu c trng ca dng
bo ch (sai s KL, th tch, bn c hc)
- Yu cu nh tnh, nh lng, tinh khit
Cng tc xy dng tiu chun thuc
Phng php xy dng yu cu k thut
1. La chn ch tiu: da vo
- YCKT
- Thc t
- iu kin KT Khng qu nhiu, qu t
Ni ln c trng CL
thuc
Ph hp /k c th
Cng tc xy dng tiu chun thuc
Phng php xy dng yu cu k thut
2. XD mc ch tiu:
Mc ch tiu: l gi tr c th hay
khong gi tr thuc phi t c
2/23/2014
8
Cng tc xy dng tiu chun thuc
2. XD mc ch tiu:
Ch tiu c sn trong quy nh:
- Kim tra xem xt li
- p dng hoc xut
Ch tiu cha c sn trong quy nh:
- Phi lm thc nghim a ra s liu
ph hp
Cng tc xy dng tiu chun thuc
2. XD mc ch tiu:
Phi tin hnh lm th vi mu t nht ly t 3 l
SX th hay 3 l s/p c QTSX n nh
S dng pp thng k (xt sai s, khong tin cy,
chnh xc)
Gii hn tin cy tm c qua th nghim cn cn
c thm /k kinh t, thc t quy nh mc ch
tiu a vo TC
Cng tc xy dng tiu chun thuc
2. XD mc ch tiu:
S/p ly t nhiu l, nhiu CSSX, nn chn ch tiu
TB tin tin:
: ch tiu TB nhiu CSSX t c
: ch tiu cao nht 1 c s t c
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
Mc ch TC ha pp th
Chn quy trnh th hoc quy trnh phn
tch khi p dng cho kt qu gn
gi tr thc nht
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
Phn loi quy trnh th
nh tnh: cc php th nhm chng minh
cht cn phn tch c mt trong mu th
Cch thc hin:
- Cc p/ nh tnh
- o thng s c trng ca cht cn th
(ph UV-VIS, IR, sc k)
- So snh vi cht chun i chiu
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
Phn loi quy trnh th
tinh khit: cc php th nhm chng
minh mu th t hay khng t mc tinh
khit
Cch thc hin:
- S dng t/c c hiu (mu sc, c...)
so snh lng tp cht c trong mu
th v mu chun, t x/ gii hn tp
c trong mu phn tch
2/23/2014
9
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
Phn loi quy trnh th
nh lng: cc php th nhm x/ hm
lng ca mu th (hoc t/p chnh ca mu)
hoc hm lng cc hot cht trong mu
em th
Cch thc hin:
-PP ha hc
-PP ha l, vt l
-PP sinh hc
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
Yu cu cht lng pp th
C tnh tin tin: pp chnh xc, chn lc cao
C tnh thc t: pp ph hp /k thc t, c
tnh kh thi cao (trang b, con ngi)
C tnh kinh t: pp t tn km m vn p
ng 2 y/c trn
C tnh an ton cao: an ton L, bo v SK
(t dng ha cht c hi, thao tc nguy
him)
0 % 100 %
chn lc vs. c hiu
c hiu
chn lc
IUPAC*
- chn lc: Mc pp c th c s dng xc
nh mt i tng phn tch c th trong hn hp hoc
nn mu m khng b nh hng t cc thnh phn
khc c c tnh tng t.
- c hiu l mc cao nht ca chn lc.
*International Union of Pure and Applied Chemistry
Pp cho php x/ ng cht cn phn tch v t chu a/h
bi s c mt ca cc cht khc trong mu th
chnh xc (Accuracy)
ng
(Trueness)
chm (lp li)
(Precision)
T (-) P (+) T (-) P (-) T (+) P (-) T (+) P (+)
= A (+) = A (-)
-Sai s:
- thu hi:
- lch chun:
- lch chun tng i:
tuyn tnh (Linearity)
Nng cht cn phn tch
i lng
tn hiu
o
nhy (Sensibility)
-Gii hn pht hin (LOD):
+ S/N: 3 ln nhiu ng nn
+ 3 ln SD mu trng
-Gii hn nh lng (LOQ):
+ S/N: 10 ln nhiu ng nn
+ 10 ln SD mu trng
2/23/2014
10
Cng tc xy dng tiu chun thuc
Phng php xy dng TC PP th
LY
MU
2/23/2014
14
Kim nghim thuc theo tiu chun
Ly mu kim nghim
Ly mu c th:
Ly mu thuc c phn liu:
- Ly ngu nhin /v bao gi t l s/p to mu ban
u:
n: s bao gi ly ra
N: s /v bao gi cui cng trong l
+ Phn thp phn < 0,5 b qua; t 0,5 tr ln thm 1 /v
+ N > 100 th n
max
30
Kim nghim thuc theo tiu chun
Ly mu kim nghim
Ly mu c th:
+ N 100 tra bng
N n
1 - 10 1
11 - 40 2
41 - 80 3
81 - 100 4
Kim nghim thuc theo tiu chun
Ly mu sn phm l cht rn (ht, bt, vin):
Trng hp mt bao gi
- Xem xt ng nht ca sn phm, nu khng
ng nht phi phn loi, ly mu ring theo tng
loi
- Mu l ht, cc cn nghin nh thnh bt (tr khi
cn x/ c ht)
- Ly mu ban u 3 v tr: trn, gia, di, trn li
thnh mu chung
Kim nghim thuc theo tiu chun
Ly mu sn phm l cht rn (ht, bt, vin):
Trng hp mt bao gi
- Chia nh u mu chung thnh mu TBTN (2 - 4 ln
lng mu th cn ly)
B
B
- Chia mu TBTN thnh mu lu v mu KN
Trng hp nhiu bao gi
Kim nghim thuc theo tiu chun
Ly mu sn phm lng
Trng hp mt bao gi
- S/p ng nht: ly mu bt k v tr no
Trng hp nhiu bao gi
- S/p cha ng nht: phi khuy u trc khi ly
mu
- Nu l chai, l nh c th ly ht th tch
Kim nghim thuc theo tiu chun
Ly mu sn phm thuc m, bt nho
- Cn khuy k, trn u cho s/p ng nht trc khi
ly mu
- Ly mu nh vi mu lng, rn
Ly mu thnh phm cha ng gi l
- L s/p c 1 2 bao gi: m c 1 hoc 2 bao gi
- L s/p c 3 bao gi: m 3 bao gi
- Ly t nht 3 mu ban u 3 v tr khc nhau ti
mi bao gi
- Trn u to mu TBTN
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15
Kim nghim thuc theo tiu chun
Ly mu kim nghim
Bao gi v dn nhn:
- Sau khi ly mu cho vo ng, ngi ly mu
bao gi, dn nhn, nim phong mu
- Phi c ch k xc nhn ca c s c ly mu
trn nim phong v bin bn ly mu
Kim nghim thuc theo tiu chun
Tin hnh kim nghim
Nhn mu:
- Mu phi c ly ng theo TT quy nh
- Mu phi c ng gi, nim phong, c nhn
thng tin cn thit (tn thuc, s l, TCYC kim tra)
- Cc mu do thanh tra ly v phi c bin bn ly mu
- Cc mu gi phi km cng vn, giy gii thiu
- Mu xin php SX phi km TL theo quy nh
- Mu nhn qua ng bu in: kim tra k nim
phong, bo li ni gi, ch KN sau khi c kin ca
ni gi mu
Kim nghim thuc theo tiu chun
Tin hnh kim nghim
Kim nghim, x l kt qu:
- Chun b TL: TCVN, TCCS
- Chun b dng c, ha cht, thit b theo y/c TC
quy nh. B tr TN hp l mu lm, trnh
nhim bn, bin cht mu
- Tin hnh phn tch theo TC
- X l s liu, a ra kt lun v mu (t, khng t)
- Ngi lm KN cn c s ghi chp y s liu khi
tin hnh TN, s ny l bn gc ca s liu cng b
trn phiu KN
Kim nghim thuc theo tiu chun
Tin hnh kim nghim
Vit phiu tr li kt qu
- Tr li bng phiu KN hoc phiu phn tch
- Phiu KN: xc nhn KQKN theo TLKT hp php ca
mt mu thuc
- Phiu phn tch: xc nhn KQPT ca 1 hay nhiu
tiu ch trong TCKT ca 1 mu thuc
KNV vit phiu tr li ni b
(cha chnh thc) , k tn
CB ph trch phng TN duyt li,
a phng chc nng
Lnh o duyt ln cui
Tr li chnh thc bng phiu
KN hay phiu phn tch
Kim nghim thuc theo tiu chun
Tin hnh kim nghim
Ni dung chnh phiu KN
- Tiu : tn CQKN, s phiu KN, tn mu KN, l lch
mu..)
- Cc ch tiu th
- Kt lun cui cng v mu c KN
- Ch vit trong phiu KN phi r rng, chnh xc, y
v thng nht
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16
Kim nghim thuc theo tiu chun
Tin hnh kim nghim
Lu mu ti CQKN
- Mu lu phi c nh s cng SK mu th
cng loi
- c s dng trong TH c tranh chp v KQ
cng b phiu KN
- Phi c lu ng thi gian quy nh (3 thng sau
khi ht HD vi mu c HD)
- S, phiu KN phi lu t nht 3 nm, hy phi c
GCQ duyt
Ni dung chnh ca GLP
Mc ch
- Xy dng /v KN p ng y y/c cng tc KTCL
thuc
- m bo KQPT thu c tin cy, c tnh php l
- Gip tra cu, tm ra nhanh chng ngun gc sai st
Ni dung chnh ca GLP
V t chc v nhn s
- Phng KN thuc phi c cc b/p chuyn mn,
hu cn, ng k, lu tr mu c chc nng nhim
v r rng, c XD, c ngi c thm quyn ban
hnh
- Nhn vin phi c o to, HL v chuyn mn
c th thc hin n/v c giao, c tinh thn trch
nhim cao
- Nhn vin phi mc trang phc theo quy nh, phi
c k/tr sc khe, khng lm nhim bn cc php
th, dng c, h thng TN
Ni dung chnh ca GLP
V c s vt cht chung
- C din tch lm vic ph hp vi y/c t ra, cho
php sp xp hp l dng c, thit b; c mi trng
tt v nh sng, thng gi, t
o
, m..
- m bo tnh bit lp: khng b nhim bn do mi
trng hay b/p ln cn, m bo v sinh theo quy
nh
- Bo m cng tc an ton, cc phng tin bo h
L, s dng, bo qun cht c, x l cht thi
Ni dung chnh ca GLP
Trang thit b
- c trang b y TTB p ng y/c th
nghim. Thit b cn c la chn, chun ha, c CL
ph hp.
- TB phi t v tr thch hp, tin cho s dng, kim
tra, bo dng
- nh k phi c hiu chun, kim nh, bo dng
- Phi c ni quy vn hnh, HDSD, s theo di SD, c
nhn chu trch nhim qun l
Ni dung chnh ca GLP
C s vt cht cho cc php th
- Tt c php th phi c quy trnh c vit chi tit v
chun ha
- Mi ha cht, TT, cht chun phi p ng ng cc
y/c quy nh
- TT, ha cht, cht chun b bin cht, qu hn
khng c php s dng
Quy nh v nguyn tc
- C s cho cc php th t, /lng, tinh khit, hot
lc, bn vng ca thuc, quy nh v mu th,TT,
cht i chiu
2/23/2014
17
Ni dung chnh ca GLP
Quy nh v quy trnh v hng dn th nghim
- Quy trnh, hng dn th nghim phi r rng, chnh
xc, c chun ha, c lnh o duyt thng qua
- KNV tin hnh TN phi bo co chi tit nhng hin
tng gp phi trong qu trnh TN vi ph trch
Quy trnh v bo co kt qu
- Phi bo co y : mc ch TN, ni TN, tn mu
th, ngy TN, pp s/d, ngi TN, pp x l s liu, KQTN,
kt lun, k xc nhn, ni lu mu lu, HS, TL
KN THUC BNG CC PP HA HC
Phng php chun acid base trong mi
trng khan
nh tnh mt s ion bng p/ ha hc
Xc nh gii hn tp cht
Cc phn ng nh tnh
T c SGK Mc ch: th tinh khit ca thuc
Tc hi ca tp cht:
- Gy hi cho sc khe
- Gy tng k ha hc: nh hng ti phm
cht, bn ca thuc
- Xc tc y nhanh qu trnh phn hy thuc (vt
kim loi, m)
- Th hin mc tinh khit cha m bo
ngha:
- Cho bit mc tinh khit ca thuc
- Cho php xem xt ngun gc gy ra tp khc
phc
Th gii hn tp cht trong thuc
Nguyn nhn gy ra tp cht:
- NL, ph liu, bn thnh phm cha tinh khit
- Quy trnh SX cha ph hp hoc cha c
thc hin nghim chnh
- Dng c s dng cha ph hp
- Phng php SX cha tt
- Pht sinh trong qu trnh bo qun do mi
trng, v sinh, cht bo qun
- Dng gian ln ca nh SX
Th gii hn tp cht trong thuc
Phng php xc nh:
-Xc nh xem cc tp cht c vt g/h cho php
khng
-Dng cc p/ bn nh lng
-Thc hin bng pp so snh
Phng php x/ g/h tp cht
2/23/2014
18
Mu th
Mu chun so
snh
(c cha tp
cn th vi s
lng g/h
cho php)
1 2
1
2
1
2
So snh c
So snh mu
Quy nh:
-Ha cht, dung mi khng c c tp cn th
-S dng cn phn tch, dng c th tch chnh
xc khi chun b mu th v mu chun so snh
-Hai ng phn ng so snh phi ging nhau
hon ton
-Thuc th cho vo hai bnh phi ging nhau v
thi gian, s lng, th tch
-So mu: nhn ngang trn nn trng
-So c: nhn t trn xung
Phng php x/ g/h tp cht
C acid - base trong mi trng khan
C s l thuyt:
Thuyt proton ca Bronsted Lowry
- Cp acid base lin hp
HA H
+
+ A
-
- P/ acid base:
Acid 1 + Base 2 Acid 2 + Base 1
C acid - base trong mi trng khan
Vai tr ca dung mi:
C th tc ng theo 2 hng
Solvat ha cht tan Solvat ha cht tan
-Dung mi c tnh acid: lm tng tnh base ca cht tan
R-NH
2
+ CH
3
COOH R-NH
3
+
+ CH
3
COO
-
-Dung mi c tnh base: lm tng tnh acid ca cht tan
HA + S A
-
+ SH
+
-Dung mi tr: solvat ha theo c ch khc (lin kt hydro,
phc , lc Van der Waals)
C acid - base trong mi trng khan
Tc ng ln qu trnh in ly ca cp ion Tc ng ln qu trnh in ly ca cp ion
-Dung mi c ln: ion to ra do solvat ha u phn ly
thnh ion t do
-Dung mi c nh: ion tn ti di dng cp ion
Qu trnh in ly ca cp ion do quyt nh
HA + S HS+A- HS+ + A-
K
i
K
d
Solvat ha in ly
C acid - base trong mi trng khan
Phn loi s b dung mi theo Phn loi s b dung mi theo
- > 50: H
2
O, formamid, dimethylsulfoxid: acid, base tn ti
ch yu di dng ion t do
- < 30: ethanol, aceton: tn ti nhiu cp ion
- < 10: benzen, cloroform, acid acetic: tn ti cp ion l ch
yu
2/23/2014
19
C acid - base trong mi trng khan
Khi nim pH:
-Trong dung mi khan, x/ pH biu kin
HS + HS H
2
S
+
+ S
-
H
2
S
+
l ion lionium, S
-
l anionlyat
pH biu kin: pH =
K
s
=
-Thang c lin quan ti hng s t in ly K
s
ca dung mi
C acid - base trong mi trng khan
Khi nim pH:
VD: 2CH
3
COOH CH
3
COOH
2
+
+ CH
3
COO
-
K
s
= [CH
3
COOH
2
+
][CH
3
COO
-
]
- di thang pH biu kin ph thuc vo K
s
:
Methanol: pK
s
= 17
Ethanol: pK
s
= 20
Acid acetic: pK
s
= 6,35
C acid - base trong mi trng khan
Xc nh im tng ng:
Ch th mu pH - Theo di s i mu ca CT
Ch th o th
- in cc SS: calomel, bc clorid
- in cc CT: thy tinh
Ch
- Khi x/ im tng ng theo di s thay i in th
- Cn trung ha dung mi trc khi chun
- Cn x l in cc CT ph hp
- Hay s/d: tm tinh th, tm methyl, CT hh
C acid - base trong mi trng khan
ng dng trong KN thuc:
- Khi cht phn tch khng ha tan trong nc
-Tnh acid, base qu yu trong mi trng nc, khng x/
c im tng ng
- Cc acid, base a chc c hng s in ly trong nc t
khc bit nhau
C acid - base trong mi trng khan
nh lng acid:
Cc cht HC c tnh acid yu:
- Acid carboxylic
- Dn xut enol, imid, sulfonamid
- Dn xut th phenol: polyclorophenol, polynitrophenol
- Hh cc cht c tnh acid hay acid a chc
- Dng dung mi base tng tnh acid ca cht phn tch
- Dung mi hay s/d: pyridin, DMF, t-BuOH (C acid
carboxylic, d/x phenol)
i tng
Dung mi
C acid - base trong mi trng khan
nh lng acid:
Cc dd chun base:
- KOH trong MeOH
- Methylat kim loi kim (natri, kali)
- Tetraalkylammonium hydroxyd
(t-Bu
4
NOH/benzen MeOH (95:5))
- Dd chun KL kim d gy sai s base cho in cc TT
- Tetraalkylammonium hydroxyd: c, pha ch lu, kh
bo qun
Dung dch chun
Ch
2/23/2014
20
C acid - base trong mi trng khan
nh lng acid:
- Acid benzonic (C6H5COOH): E = M = 122,12
- Acid succinic (CH2COOH)2: E = M/2 = 59,05
- Acid sulfamic (NH2SO3H): E = M = 97,09
- Kalihydrophtalat, E = M = 204,22
Cht chun
C acid - base trong mi trng khan
nh lng base:
Cc alkaloid, base nit tng hp
i tng
Dung mi
- Dng dung mi acid tng tnh base ca cht phn tch
- Dung mi hay s/d: AcOH, anhydrid acetic (khng dng
/l amin bc 1,2), MeCN
C acid - base trong mi trng khan
nh lng base:
- HClO
4
trong AcOH khan
- HClO
4
trong 1,4-dioxan
Dung dch chun
- Kalihydrophtalat, E = M = 204,22
Cht chun
Phn ng chun
- Solvat ha: RNH
2
+ CH
3
COOH RNH
3
+
CH
3
COO
-
- Trung ha:
RNH
3
+
CH
3
COO
-
+ HClO
4
RN
+
H
3
Cl
-
O4 + CH
3
COOH
C acid - base trong mi trng khan
nh lng mui:
Mui ca cc acid yu hn AcOH BH
+
Y
-
- Y
-
: propionat, maleat, benzoat, salicylat
- BH
+
Y
-
c C trc tip nh 1 base bng HClO
4
- Y- c trung ha bng HClO
4
, p/ khng c hiu
Mui ca cc acid mnh hn AcOH BH
+
X
-
- X
-
: halogenid, sulfat
- Halogenid: X
-
qu yu, khng p/ ton lng c
vi HClO
4
Pp Pifer - Wollish
2BH
+
X
-
+ Hg(CH
3
COO)
2
2CH
3
COO
-
BH
+
+ HgX
2
2CH
3
COO
-
BH
+
+ 2HClO
4
2CH
3
COOH + 2BH
+
ClO
4
-
Pp Billon
- Ha tan mui trong ethanol, BH+ l acid mnh c th C
bng NaOH 0,1N
-Thm HCl d chuyn ht B (nu c trong BH+X-) thnh
BH+
B + HCl BH
+
+ Cl
-
HCl + NaOH NaCl + H
2
O
BH
+
X
-
+ NaOH NaX + B + H
2
O