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B Y T
Li gii thiu
Thc hin mt s iu ca Lut Gio dc, B Y t ban hnh
chng trnh khung o to trung cp ngnh Y t. B Y t t chc bin
son ti liu dy - hc cc mn c s v chuyn mn theo chng trnh
trn nhm tng bc xy dng b sch chun trong cng tc o to
trung cp y t.
Sch KIM NGHIM THUC c bin son da trn chng trnh
gio dc ngh nghip ca B Y t bin son trn c s chng trnh
khung c ph duyt. Sch c cc tc gi Nguyn Th Kiu Anh,
Trn Tch, V Th Thu Thu bin son theo phng chm: Kin thc c
bn, h thng; ni dung chnh xc, khoa hc; cp nht cc tin b khoa
hc, k thut hin i v thc tin Vit Nam. Sch c cu trc gm
22 bi bm st theo chng trnh gio dc vi nhng ni dung theo
hng dn chun quc gia. Ti liu l tin cc gio vin v hc
Sch KIM NGHIM THUC c Hi ng chuyn mn thm nh
sch v ti liu dy - hc trung cp v dy ngh ca B Y t thm nh
vo nm 2007. B Y t quyt nh ban hnh lm ti liu dy - hc chnh
sch phi c chnh l, b sung v cp nht.
B Y t xin chn thnh cm n cc tc gi v Hi ng chuyn mn
thm nh u t cng sc hon thnh cun sch; Cm n PGS. TS.
Trnh Vn Lu, TS. Phng Th Vinh c v phn bin, cun sch
sm hon thnh kp thi phc v cho cng tc o to nhn lc y t.
Ln u xut bn, chng ti mong nhn c kin ng gp ca
ng nghip, cc bn sinh vin v cc c gi ln xut bn sau c
hon thin hn.
V K
A C V
- B Y
Bi 1
I CNG V CNG TC KIM TRA
CHT LNG THUC, M PHM
MC TIU
- Trnh by c s cn thit phi kim tra cht lng thuc.
- Bit c ni dung, h thng t chc kim tra cht lng thuc ca
Vit Nam.
2) C s nh xng.
3) hit b.
4) V sinh.
5)
6) hao tc sn xut.
7) Dn nhn v ng gi.
8)
9) thanh tra.
10)
s phn phi.
3) C s vt cht.
4) hit b phn tch v hiu chnh thit b phn tch.
5) huc th v cht i chiu.
6) iu chun cht lng v phng php phn tch.
7) Mu th.
8) h nghim v nh gi kt qu.
9)
s ti liu.
3) V sinh.
4) Cc quy trnh bo qun.
5) huc tr v.
6)
7)
s ti liu.
- Phi hp vi thanh tra B Y t thc hin chc nng kim tra, thanh
tra nh nc v cht lng thuc v x l vi phm php lut v cht
lng thuc theo thm quyn.
2.1.2. C quan qun l nh nc v cht lng thuc a phng
S Y t ch o qun l ton din v cht lng ca thuc a
phng (thng u quyn cho phng nghip v Dc) c nhim v:
- Ph bin, hng dn v t chc thc hin cc vn bn php lut
v qun l cht lng thuc ti a phng.
- hc hin chc nng kim tra, thanh tra nh nc v cht lng
thuc v x l vi phm v cht lng thuc trong phm vi a phng.
2.2. H thng kim tra cht lng thuc
2.2.1. C quan kim tra cht lng ca Nh nc v thuc
- rung ng l Vin Kim nghim trung ng (
Kim nghim thnh ph Ch Minh.
i) v Vin
am v thuc.
T LNG GI V BI TP
1. Mc tiu ca cng tc kim tra cht lng thuc. Cc yu cu c
bn t mc tiu trn.
2. i dung chnh ca cng tc kim tra cht lng thuc. iu kin
thuc c a vo lu thng, phn phi, s dng.
10
am gm:
am gm:
Ch Minh.
11
Bi 2
CNG TC TIU CHUN HO V
KIM NGHIM THUC THEO TIU CHUN
MC TIU
- Trnh by c ni dung ca cng tc tiu chun ho.
- Trnh by c 3 ni dung chnh ca cng tc kim nghim thuc
theo tiu chun (ly mu, tin hnh kim nghim, nh gi kt qu v
vit phiu tr li).
12
am, iu chun
am v
13
am)
14
15
16
17
4) V nhit : Dng thang bch phn, k hiu oC. Khi khng ghi
c th, quy c:
hit chun
20oC
hit thng
20 - 30oC
c m
40 - 50oC
c nng
70 - 80oC
c cch thu
98 - 100oC
hit ni bo qun:
< -10oC
t lnh
Lnh
2 - 10oC
Mt
10 - 20oC
20 - 35oC
hit phng
20 - 25oC
35 - 40oC
> 40oC
t nng
ung
thm
trng
C
C
C
18
19
20
Hnh 1. S ly mu thuc
Sau khi ly mu xong, ngi ly mu t tay dn nhn nim phong,
bao gi (phi c ch k xc nhn ca ngi ly mu v c s c ly
mu) v bin bn ly mu (cng phi c ch k xc nhn).
b) Ly mu c th
Cn c vo l thuc phi ly mu, xem xt phn loi tin hnh ly
nh sau:
- Ly mu thuc c phn liu (l sn phm thuc dng thuc c phn
liu):
l sn phm ly ra cc n v bao gi mt cch ngu nhin bt
k: Cc gi c ly ra phi c lp vi d kin ca ngi ly mu
(khng nn la chn theo cm quan ly mu xu hay mu tt). L thuc
phi ng nht, hp l v s lng hay khi lng (V d khng qu
500.000 vin vi thuc vin, khng qu 50.000 ng vi dng ng,...). S
bao gi trong l ly ra to mu ban u tnh theo cng thc:
21
+ Khi tnh theo cng thc trn, nu phn thp phn nh hn 0,5 b
qua, nu ln hn 0,5 th tng thm mt n v.
+ Khi
+ Khi
1 - 10
11 - 40
41 - 80
81 - 100
22
nu trn.
- Ly mu l sn phm lng:
+ rng hp mt bao gi: u sn phm l ng nht th ly mu
bt k v tr no cng c. u khng ng nht, trc khi ly mu phi
khuy u, sau mi ly mu.
+ rng hp nhiu bao gi: ly theo cng thc:
u l nhng chai l nh th c th ly ht th tch.
- Ly mu l cc sn phm thuc m, bt nho:
in hnh ly mu nh cc sn phm lng nhng ch khuy k,
trn u c hn hp ng nht, sau mi ly mu.
- ng gi v dn nhn:
Sau khi ly mu v cho vo ng, ngi ly mu ng gi, dn
nhn v nim phong mu, lm bin bn ly mu. Lu phi c ch k
xc nhn ca c s c ly mu nhn nim phong v bin bn ly
mu.
2.2. Tin hnh kim nghim
2.2.1. Nhn mu
B phn nhn mu ca c quan kim nghim phi kim tra xem mu
c p ng cc yu cu khng (cn nim phong khng, c thng
tin khng,...).
2.2.2. Kim nghim, x l kt qu
Cng vic ny do b phn k thut thc hin. hng thng gm
cc ni dung sau:
- Chun b ti liu: theo CV
hoc C.
23
T LNG GI V BI TP
1. i dung chnh ca cng tc tiu chun ho.
2. rnh by phng php xy dng tiu chun v yu cu k thut.
V phng php th. Yu cu cht lng i vi mt phng php
th.
3. i dung chnh ca cng tc p dng tiu chun trong thc t.
4. rnh by mt s quy nh chung khi s dng Dc in Vit
(dng trong cng tc kim nghim thuc).
24
am
B. 2
C. 3
D. 4
B. 2
C. 3
D. 4
B. 2
C. 3
D. 4
B. 2
am
C. 3
D. 4
quy nh v nhit :
hit thng l:
A. 20oC
80oC
B. 20 - 30oC
D. 40 - 50oC
25
C. 70 -
b)
c nng c nhit l:
A. 60oC
80oC
c)
B. 50 - 65oC
D. 100oC
C. 70 -
10. Dc in Vit
a)
am
B. 65 - 75oC
D. 105oC
C.
quy nh:
B. 100,5%
D. 102,0%
C.
B. 0,4mg
26
C. 0,3mg
Bi 3
PHNG PHP X L S LIU, TNH TON
V TR LI KT QU KIM NGHIM
MC TIU
- Trnh by c ba loi sai s v cch hn ch cc sai s ny trong
kim nghim.
- Tnh c sai s ca kt qu thc nghim.
- Bit cch ghi chp, trnh by kt qu thc nghim v phiu kim
nghim.
- Trnh by c nm cch x l mu thng dng trong kim
nghim.
Gi tr trung bnh
l ng tin cy hn c v
c ly lm kt qu ca php xc nh.
i tr trung bnh thng khc vi gi tr thc
xc nh, s sai khc ny chnh l sai s ca php xc nh.
Kt qu ca php xc nh c nh gi chnh xc ( ng
v chm).
+ ng phn nh s ph hp gia kt qu thc nghim thu c
(
+ chm ( lp li) phn nh s ph hp gia cc kt qu thu
c (x1, x2,... xn) trong cc th nghim cng iu kin quy nh ca
php xc nh (gi l cc php xc nh song song).
C th biu th sai s di dng sai s tuyt i v sai s tng i.
+ Sai s tuyt i:
27
28
- nh gi tr trung bnh:
t
0,95
12,7 4,3 3,2 2,8 2,6 2,5 2,4 2,3 2,3 2,2 2,1 2,0
t
0,99
63,7 9,9 5,8 4,6 4,0 3,7 3,5 3,4 3,3 3,2 2,8 2,6
29
10
20
Ln
K=n-1
hay
h vy bin gii tin cy hay cn tin cy, hoc gii hn tin cy l gii
hn hai bn ca
* Sai s tng i l
V d:
Kt qu nh lng cht XC (g/l) ca 5 th nghim cng iu kin
ca mt mu th l: 2,25; 2,19; 2,11; 2,38; 2,32.
- nh sai s tng i ca php nh lng?
Gii:
- nh gi tr trung bnh:
- nh lch chun:
- Kt qu xc nh:
30
31
i sn xut.
32
5) S l, hn dng.
6)
gi v ni gi mu.
9) S ng k kim nghim.
10)
gi nhn mu.
33
149,6mg
160,1mg
158,0mg
156,9mg
147,8mg
162,3mg
154,5mg
159,4mg
160,3mg
149,2mg
157,2mg
151,9mg
152,6mg
155,3mg
160,8mg
153,9mg
158,3mg
156,1mg
.
Kt lun: t yu cu.
d) r
34
TB
= 0,15622g.
- Cn bt vin: mT (g).
- Ho tan mT bng hn hp (bao gm 100 ml nc v 10 ml dung
dch acid acetic 1M) trong bnh nh mc 100 ml.
- Lc.
- 50,0 ml dch lc +1 ml dung dch h tinh bt. nh lng ht V ( ml)
dung dch iod 0,1N c K = 1,0033.
m lng X (%) acid ascorbic trong ch phm so vi hm lng
ghi trn nhn c tnh theo cng thc sau:
Kt qu:
Ln
mT (g)
0,3165
0,3123
0,3140
V ( ml)
11,30
11,20
11,25
X (%)
98,56
99,00
98,90
Kt lun: t yu cu.
35
C
V
AM
am
Kt qu
ng
t
t
4. r: Khng qu 15 pht
5. nh lng: m lng acid ascorbic (C6H8O6
110,0% so vi lng ghi trn nhn.
36
t
(98,82%)
Ln 2
Ln 3
Ln 4
Ln 5
0,0271
0,0282
0,0279
0,0271
0,0275
0,95.
5. in cm t cn thiu vo ch trng trong cu di y:
Phng php thng thng x l mu gm: o tan
mu,........................(A)............................, phn hu mu bng k
thut vi sng, phn hu bng nhit, x l mu bng k thut tch
pha. Phng php phn hu bng nhit dng phn
hu...............(B)............... Phng php ny c th thc hin bng
cch...........(C)............... trn ngn la hoc.......(D)................ trong
l nung.
6. rnh by ni dung chnh ca mt phiu kim nghim.
37
Bi 4
DUNG DCH CHUN, DUNG DCH ION MU,
THUC TH, CH TH MU
THNG DNG TRONG KIM NGHIM
MC TIU
- Trnh by c cch pha cc dung dch chun, dung dch ion mu,
thuc th, ch th mu thng dng trong kim nghim thuc.
- Tnh c h s hiu chnh ca dung dch chun khi pha bng
cc phng php khc nhau.
38
39
rong :
a: lng cht gc cn, tnh bng g.
: chun l thuyt ca dung dch mi pha tnh theo cht gc, tnh
bng g/ ml.
V: th tch dung dch chun dng, tnh bng ml.
V d: Pha v xc nh nng dung dch chun
Na2S2O3.5H2 (khng phi l cht gc).
a 2S2O3 0,1
40
rong :
C0 l nng ng lng l thuyt.
V0 l th tch (tnh bng ml) v K0 l h s hiu chnh ca dung dch
chun dng chun ho.
C: nng ng lng l thuyt ca dung dch chun cn pha.
V: th tch dung dch chun cn xc nh h s K, tnh bng ml.
V d: Pha v xc nh nng dung dch chun
NaOH.
0,1
V a
d ht m v d b carbonat ho nn khng tho mn yu
cu cht gc, do pha dung dch chun a
c nng xp x 0,1
bng cch: o tan 4,50g a
trong 5 ml nc. y kn bnh cha
bng nt cao su, yn 1 ngy ri gn ly dung dch trong pha trn v
pha long vi nc ct mi un si ngui n va 1 lt, trn u.
Sau xc nh li nng dung dch a
bng dung dch Cl 0,1
c K = 0,9985 nh sau: Ly chnh xc 20,0 ml dung dch a
41
t ng chun Ag
0,1N c
42
43
3C
44
3.
Dng loi tinh khit phn tch c cha hm lng kim ton phn
khng nh hn 97% tnh theo a
v khng c c qu 2,0%
Na2CO3. atri hydroxyd c dng cc trng hay thi hnh tr, d ht m.
Bo qun trong ng kn.
* Dung dch natri hydroxyd xM (xN): Ho tan 40x (g) natri hydroxyd
trong nc v thm nc va 1000 ml.
* Dung dch natri hydroxyd long: Ho tan 8,5g natri hydroxyd trong
nc v thm nc va 100 ml.
3.2. Thuc th
3.2.1. Thuc th Nessler
45
46
3,0 () n p
4,4 (vng).
47
4,4 () n p
6,0 (vng).
6,8 (vng) n p
8,4 ().
48
H4.
4.
b) en eriocrom .
c) phenol.
d) Kali cromat.
f) tinh bt.
e) Phenolphtalein.
49
B. 3,5 4,5
B. 4,4 6,0
B. 3,5 4,5
50
C. 2,8 3,5
D.
C. 4,8 5,5
D.
C. 6,5 7,8
D.
t:
t:
t:
51
Bi 5
MT S PHNG PHP PHN TCH
HO L DNG TRONG KIM NGHIM
MC TIU
- Trnh by c khi nim chung v phng php tch v sc k,
ng dng sc k lp mng trong kim nghim.
- Trnh by c nguyn tc ca phng php o th, ng dng o
pH v chun o th.
- Trnh by c nguyn l c bn ca phng php o quang ph
hp th UV-VIS v ng dng nh tnh, nh lng.
52
53
54
C ch tch
ca cc cht
Kh
Ct
p ph
Kh - lng
Kh
Lng
Ct
Phn b
Lng -
Lng
Ct
p ph
Lng - Lng
Lng
Lng
Ct
Phn b
Lng i
Lng
Ct
rao i ion
Lng
Lp mng
p ph
Lng
Lng
Lng
Kh -
p ph
Cch b tr
pha tnh
ha trao
Lp mng
iy
y (sc k
el)
iy sc k Phn b
Ct
55
g nh tnh, th
tinh khit, cng c th nh lng. u im c bn l thit b n
gin, thi gian phn tch nhanh, kh chn lc.
b) i lng c trng
h s lu gi
(Retard factor)
khng lp li do ph thuc
nhiu yu t kh kim sot nh: cht lng v hot tnh ca cht hp
ph, m ca cht hp ph, cht lng ca dung mi,... Do ngi
ta thng dng h s lu gi tng i td.
f
( nh gi kh
rong :
dA, dB: l khong cch t im xut pht n tm ca vt sc k ca cht
A v cht B trn sc (A v B l 2 cht trong cng hn hp, d B> dA).
DA, DB l ng knh ca vt sc k ca cht A v B trn sc .
Yu cu:
> 1, gi tr ti u
= 1,5.
56
t ca
cht nghin cu. Dung mi c th l n hoc hn hp. Cc dung mi
phi t tinh khit cao.
ph hp v c np y kn.
micropipet hay ng mao qun thng, ng mao qun nh mc chnh
xc.
quang t ngoi, my o mt vt.
d) Cc bc tin hnh
ph hp vi yu cu phn tch, iu ch va ca cht hp ph, tri bn
mng, lm kh t nhin, hot ho bn mng 105 oC 110oC.
kh trong bnh bng cch lt giy lc xung quanh thnh trong ca bnh,
pha dung mi (lng dung mi s dng sao cho sau khi thm u vo
giy lc, cn li 1 lp dy 5 10mm y bnh). y np bnh v yn
1 gi.
mu khng qu nh v khng qu ln (thng thng 0,1 tch 0,001 - 0,005 ml). im chm xut pht phi cch mp di bn
mng 1,5 - 2,5cm v cch b mt dung mi 0,8 - 1,0cm. Vt chm phi
nh gn (ng knh 2 6mm), cc vt chm cch nhau 15mm, vt
chm cch b bn ca bn mng t nht 1cm.
k (cc vt chm phi trn b mt ca lp dung mi). y kn bnh v
yn nhit c nh. hng khi ng i ca dung mi c 10 12cm th kt thc giai on trin khai sc k.
Lm bay hi dung mi cn ng li trn bn mng. Pht hin vt sc k
bng phng php ho hc hoc ho l (hin mu bng phun thuc th
hoc dng n UV 254nm v 366nm). Quan st mu vt, o v tnh f
(hoc td, RS).
kt qu trn rt ra kt lun v nh tnh, th tinh khit theo yu
cu ca php phn tch. nh lng c th da trn din tch, m
mu ca cc vt hoc x l bng cc bin php ho hc thch hp ly
cht nghin cu ra khi bn mng.
57
+ Bnh chy sc k.
+ ng ong, ci chy s, tha s.
+ ng mao qun.
+ Bnh ng iod lm hin mu.
+ Dung dch chun morphin 0,5%.
+ Dung dch chun papaverin 0,5%.
+ Dung dch hn hp morphin v papaverin (dung dch bi tp).
+ Cloroform, aceton, methanol, amoniac c, iod tinh th, silicagen,
thch cao.
58
f,
nh tnh ng.
+ Vi anionid:
59
V d: nh lng
- Nguyn tc:
Da trn phn ng trao i thun nghch gia cc ion trong dung
dch cht nghin cu vi cc ion trong mt cht gi l ionid. Qu trnh
trao i tun theo nh lut tc dng khi lng.
i vi a2SO4, khi cho dung dch chy qua ct trao i ion (cha
cationid dng +) trong ct s xy ra phn ng:
2RH + Na2SO4 = 2RNa + H2SO4
Dung dch chy t ct ra l 2SO4, em nh lng dung dch 2SO4
ny bng dung dch a
bit nng , suy ra c hm lng
Na2SO4 c trong mu phn tch.
- Dng c, ho cht:
+ Ct trao i ion (dng Buret).
+ ng nghim nh.
+ Cationid (loi trao i acid mnh).
+ Dung dch Cl 0,1 .
+ Ch th da cam methyl.
+ Dung dch chun
0,1 .
60
chy
-von (k hiu l
eV) hoc kC/mol (1eV = 23 kCal/mol).
- n s nh sng l s dao ng hon chnh m sng thc hin
c trong 1 giy.
185 400nm
61
Vng kh kin:
400 760nm
700
760 630nm.
Cam:
630 600nm.
Vng:
600 570nm.
Lc:
570 500nm.
Lam:
500 450nm.
Chm:
450 430nm.
Tm:
430 400nm.
62
vi K l h s hp th.
c gi l h s
= D khi C = 1mol/l v l = 1cm) c trng cho bn
cht ca cht nghin cu trong dung dch ch ph thuc vo bc sng
nh sng n sc.
+ u C tnh theo % (KL/ ) ta c: D = E1%1cm.C.l v E1%1cm l h s
hp th ring (h s tt ring).
truyn qua thp, mt quang cao v ngc li.
3.2.2. iu kin p dng nh lut
- nh sng phi n sc.
-
63
64
ml.
- Tin hnh:
Pha long dung dch tim vitamin B12 c nng khong 0,0025%
ml). Qut ph hp th ca dung dch cc bc sng t 200nm
n 650nm, dng cuvet thch anh c b dy 1cm, mu trng l nc
ct.
:
+ m cc cc i hp th. i chiu vi l thuyt kt lun.
65
hay n D2 (deuterium).
3.4.2. B n sc ho
him v ch yu l to ra tia n sc.
- u my dng knh lc mu, knh tt nht cng ch c th t c
mc n sc 10nm.
66
67
rong :
D: i tr mt quang o c ca dung dch th vitamin B12 207:
hp th ring (E1%1cm) ca vitamin B12 bc sng 361nm.
n:
da vo ng chun
xc nh CX.
Yu cu:
Hnh 7. th biu din mi
quan h
ca mt quang vo nng
68
3)3
0,01M).
69
70
D0
.C0.l
Cx cn xc nh (cng iu kin
.Cx.l
tnh c
71
+ Bnh gn 50 ml.
+ Bnh nh mc 25 ml.
+ Cc thu tinh.
+ Phu lc, giy lc.
+ ng nghim to.
+ Dung dch novocain chun 1mg/ ml (0,1%).
+ Dung dch tim novocain nh lng (khi dng phi tnh pha
long c nng gn chun).
+ Dung dch m acetat (p
= 4,20).
72
rong :
Cx: nng dung dch novocain cn nh lng (mg/ ml).
Cch: nng dung dch novocain chun (mg/ ml).
: mt quang trung bnh ca bnh X1 v X2.
: mt quang trung bnh ca bnh S 1 v S2.
Ch : Khi o mt quang ca dch chit khng c s dng
cuvet nha.
3.5.4. Phng php thm
x
cn xc nh c Dx
.Cx.l
mt quang Dx + t
vo dung dch cn xc nh v o
.(Cx + Ct).l.
tnh c
73
- Dng c, ho cht:
+ My quang ph UV-VIS.
+ Cn phn tch.
+ Ci, chy s.
+ Bnh nh mc.
+ Cc thu tinh.
+
iy lc bng xanh.
+ Phu lc.
+ Pipet chnh xc.
+ Berberin hydroclorid dng lm chun.
+ Mu vin nn berberin.
- Tin hnh:
+ Pha dung dch berberin 0,1% (dng lm chun): Cn chnh xc trn
cn phn tch mt lng cn thit pha (qua tnh ton), ho tan bng
nc nng.
+ Cn chnh xc 20 vin nn berberin cn nh lng. nh khi
lng trung bnh ca mt vin. ghin trong ci s thnh bt mn.
+ Cn chnh xc m gam mt lng bt vin (tng ng vi khong
0,05g berberin) cho vo cc c m loi 100 ml, tm t bt bng 10 ml
nc ct. hm 60 ml nc nng, khuy k. lng ngui 15 pht, gn
chuyn dung dch vo bnh nh mc 100,0 ml. Phn cn li thm tip
nc nng, khuy k, sau tp trung ht vo bnh nh mc 100,0 ml
trn, thm nc n vch, lc k. Lc qua giy lc kh, b 20 ml nc
lc u. Ly chnh xc 1,00 ml dch lc cho vo bnh nh mc 100,0 ml
khc, thm nc n vch. Lc k. em o mt quang bc sng
345nm vi dung dch so snh l nc ct c D x.
+ Song song tin hnh mt th nghim nh trn nhng sau khi cn
chnh xc m gam bt vin, cho thm mt lng chnh xc dung dch
chun berberin 0,1% (10,00 ml dung dch berberin chun 0,1% tng
ng 0,01g berberin) vo trc khi ho tan, cc giai on sau tin hnh
tng t. Kt qu o mt quang c D'x.
74
Dx, D'x v lng berberin chun bit thm vo, tnh hm lng
berberin trong mt vin.
4. PHNG PHP O TH
4.1. Khi nim
cc ion ca cht nghin cu da vo s o in th ca dung dch cha
cc ion .
ca phng php o th l o sut in ng ca mt
pin to bi mt in cc c th thay i ph thuc vo nng ion ca
cht nghin cu trong dung dch (gi l in cc ch th) v mt in cc
c th khng thay i (gi l in cc so snh).
C hai in cc c nhng vo dung dch phn tch. Khi ta c:
Ex = Ess - Ect
rong :
Ex l in th ca dung dch th.
Ess l th in cc so snh.
Ect l th in cc ch th.
Hnh 8. S mch o th
bt c ion no nu tm c in cc ch th tng ng cho ion .
75
heo cc nh ho hc quy c:
+ Catod ( xy ra qu trnh kh, tc l xy ra s nhn e) v cc
thng tin lin quan vit bn tri.
+ Anod ( xy ra qu trnh oxy ho, tc l xy ra s cho e) v cc
thng tin lin quan vit bn phi.
+
||.
4.2. Mt s in cc thng dng trong phng php o th
4.2.1. Cc in cc ch th
L cc in cc c in th ph thuc vo nng ca ion cht
nghin cu. V d:
+
dng o p ):
76
|)
Ag
3:
= EoAg + 0,059lg[Ag+]
AgX
= [Ag+] [X ]
4.2.2. Cc in cc so snh
L cc in cc c th khng i trong sut qu trnh o. V d:
77
2Cl2
4.2.3. Cc in cc t hp
cho gn v thun tin cho ngi s dng, hin nay cc hng sn
xut cc in cc t hp l mt in cc kp gm mt in cc ch th
v mt in cc so snh:
Calomel.
h Ag/AgCl.
- Calomel.
Cc in cc ny thng c cu to ng trc, in cc so snh bao
quanh in cc ch th.
4.3. S dng my o th o pH v chun o th
4.3.1. o pH
so snh l
calomel.
0,05 p (hoc 0,003V).
78
- Nguyn tc:
S dng my o th vi in cc ch th l thu tinh v in cc so
snh l calomel (hay Ag/AgCl) hoc in cc t hp.
hng nm iu chnh chnh ca my o th (p
metre):
= 7,00; p
+ Ch th mu vn nng.
79
= 4,00, p
= 9,00.
- Tin hnh:
+ iu chnh nm 1 my ch o p , iu chnh nm 2 n
nhit ph hp.
+ Dng giy ch th th dung dch cn o xem p
s dung dch bi tp c p khong 5.
khong no.
80
3PO4
81
+ Buret.
+ Cc ng dung dch.
+ in cc: thu tinh + calomel (hay cc tng hp).
+ Dung dch NaOH 0,1N.
+ Dung dch cn nh lng
3PO4
- Tin hnh:
+ Ly chnh xc 10,00 ml H3PO4 cn nh lng cho vo cc 250 ml
t trn my khuy t. hm que khuy lp in cc v ni vi my (ch
in cc cch y cc khong 2cm trnh que khuy chy lm v
in cc). hm nc ct cho ngp in cc. dung dch a
0,1
ln trn buret.
+ Bt my o ch o th E (mV) hoc o p .
ban u.
hi gi tr th E
+ Bt my khuy t, nh a
0,1 t buret xung, sau mi ln
thm 1 ml NaOH 0,1N
ml) tt my khuy, ghi th E. heo di
cho n khi thy c hai bc nhy th, ghi nh th tch a
0,1
tng ng vi ln cn 2 im ny (im tng ng).
+ Lp li ng tc chun trn, nhng ln cn 2 im tng
ng thm d qua chun
ml), li tt my khuy v ghi gi tr th ca dung dch. Kt qu ghi vo
bng nh sau:
VNaOH ( ml)
E (mV)
82
3PO4.
T LNG GI V BI TP
1. y nu cc phng php tch cc cht bng phng php chit.
2. rnh by nguyn tc, i lng c trng, cch tin hnh ca sc
k lp mng.
3. u nguyn tc, cch tin hnh ca sc k trao i ion.
4. in t hoc cm t cn thiu vo ch trng trong cu sau:
a) Phng php lc l phng php dng tch........................
khi pha rn.
b) Phng php ly tm l phng php dng.................... lm
lng kt ta xung.
c) Phng php chit l phng php dng............................
tch ly mt cht (hay mt nhm cht) t mt hn hp nghin
cu trong dung dch.
5. rnh by nh lut c bn v s hp th nh sng: nh lut
Lambert-Beer.
6. rnh by khi nim v ng dng ca quang ph hp th UV-VIS.
7. Cc b phn chnh ca my o quang ph UV-VIS.
8. y nu cc k thut xc nh nng dung dch trong phng
php o quang.
83
y nu mt s in cc ch
y nu mt s in cc
bng my o th.
B. 220 350nm
C. 200 400nm
D. Ln hn 200nm
B. 400 760nm
C. 300 800nm
D. Ln hn 400nm
84
A. 570 500nm
B. 760 630nm
C. 500 450nm
D. 450 430nm
B. 760 630nm
C. 430 400nm
D. 450 430nm
B. 760 630nm
C. 430 400nm
D. 450 430nm
B. Da cam
D. Vng
C. Lc
b) Mu lc vng ph vi mu:
A.
Tm
B. Da cam
D. Vng
C.
B. Xanh lam
D. ta
C.
c) Mu vng ph vi mu:
A.
Tm
Bi 6
XC NH GII HN TP CHT
TRONG THUC V TRONG DC LIU
MC TIU
- Trnh by c phng php xc nh gii hn tp cht trong thuc.
- Trnh by c cch xc nh gii hn tp cht, t l vn nt trong
dc liu.
85
86
87
ml dung dch A pha long bng nc cho 100,0 ml. Dung dch ny c
cha
(tng ng 0,005mgCl-/ ml hay dung dch
0,0005% hoc 5 phn triu).
1.2.3. Pha dung dch th
pha, gi thit mu em kim tra c cha mt lng tp cht cho
php ti a, t tnh h s pha long thch hp, sau tin hnh pha
theo tnh ton ny.
V d: Pha dung dch th tp Cl trong paracetamol (theo tiu
chun Cl khng c qu 0,01%):
V dung dch mu Cl- khi em th l dung dch c cha 0,0005% (hay
5 phn triu). Do h s pha long dung dch th s l
c cch pha nh sau: Cn 1,000g paracetamol ho tan trong nc cho
20,00 ml lc. Ly 10,00 ml dch lc em th v so snh vi 10,00 ml
dung dch mu chun Cl - 0,0005%.
rong Dc in hoc C c ghi r cch pha dung dch th l
da trn c s cch tnh ny, ngi lm kim nghim lm theo ch dn
khng cn phi tnh ton.
1.3. Mt s thuc th trong cc phn ng ho hc xc nh gii
hn tp cht
Mt s thuc th xc nh gii hn tp cht thu c sn phm
phn ng v hin tng quan st pht hin c trnh by trong
bng 6.
Bng 6. Kt qu xc nh gii hn ca mt s tp cht
88
Ion cn th (tp
cht)
Thuc th
Cl-
AgNO3
SO42-
BaCl2
NH4+
Nessler
Ca2+
(NH4)2C2O4
Arsen
Zn + HCl
Sn phm
Hin tng
quan st
a trng
BaSO4
a trng
Mu vng (nu
nhiu c mu
nu )
CaC2O4
AsH3
- Na2S (H2S)
a trng
iy tm gCl2
chuyn t vng
sang nu
en hoc nu
- Thioacetamid
St
Acid mercaptoacetic
Feri mercaptoacetat
Mu hng
Acid
sunfosalicylic
Ferisulfisalicylat
nu hay
vng
Mu vng rm
(tan trong
CHCl3)
8hydroxyquinolin
Nhm
(oxiquinolat nhm)
Magnesi
8hydroxyquinolin
Oxiquinolat Mg
Phosphat
Sulphomolybdic
(NH4)3H4[P(Mo2O7)6] Mu vng
Km
K4[Fe(CN)6]
K2Zn3[Fe(CN)6]2
Mu vng (tan
trong CHCl3)
a trng
1.4. Mt s v d p dng
1.4.1. Th gii hn tp cht amoni
C 2 phng php th gii hn tp cht amoni, chng ti ch trnh
by phng php A l phng php hay c s dng trong php th
ny.
in hnh ng thi phn ng hai bnh nh sau:
89
90
).
91
92
rong :
2.2. Ch
trn cha phn bit c, khi c th phi lm cc phn ng ho hc,
dng knh hin vi, dng cc phng php vt l, ho l khc,... pht
hin ra tp cht v vy khi tnh phi tnh c cc tp cht loi ny.
t v qu nh va khong 20g.
93
- St.
- Amoni.
- Sulfat.
- Phosphat.
94
Bi 7
PHNG PHP CHUNG
XC NH MT S CH S VT L
MC TIU
- Trnh by c phng php xc nh: khi lng ring, t trng, ch
s khc x, gc quay cc v gc quay cc ring, nhit nng chy.
- Bit cch th r v ho tan ca vin nn, vin nang.
1. KHI LNG RING V T TRNG
1.1. nh ngha
Khi lng ring l khi lng ca mt n v th tch cht xc
nh nhit t:
rong :
95
+ Lau sch t trng k bng ethanol hoc ether. Dng a thu tinh
trn u cht lng cn xc nh.
+ t nh nhng t trng k vo cht lng (khng c chm vo
thnh hoc y bnh ng). iu chnh nhit v 20 oC.
+ c kt qu khi t trng k n nh.
96
* Vi cht nh hn nc:
+ u k (alcoholmeter): hng thng cho bit cn tc l hm
lng % ( / ) ca cn em xc nh.
1.3. Phng php xc nh t trng d20 ca m, sp, nha, nha
thm
+ nh kt qu:
Ch : Khi ly kt qu xc nh:
cnomet cho kt qu vi 4 s l.
- 3 s l.
2. XC NH CH S KHC X
2.1. Khi nim
97
Ch s khc x
cht so vi khng kh l t s gia sin
ca gc ti (i) v sin ca gc khc x
( ) ca chm tia sng chiu t khng
kh vo cht .
, bit
tnh c n =
. sin
1),
98
ng vi nc ct n = 1,333 th C1%ng = 0%
n = 1,381 th C1%ng = 30%
n = 1,530 th C1%ng = 95%
3. XC NH GC QUAY CC V GC QUAY CC RING
3.1. Khi nim
nh sng t nhin l cc dao ng sng xy ra theo mi hng
trong mt phng vung gc vi phng truyn sng.
nh sng phn cc l nh sng trong cc dao ng sng xy ra
theo mt hng nht nh trong mt phng vung gc vi phng
truyn sng. Mt phng cha dao ng sng c gi l mt phng
phn cc.
phng hay s khc x qua cc mi trng (khi chiu nh sng t nhin
ti b mt ca mi trng vi gc ti m tia ti v tia phn x to thnh
gc 900 th lc tia phn x tr thnh phn cc, mt phng ti l mt
phng phn cc).
hoc dung dch), cht ny c kh nng lm quay mt phng ca nh
sng phn cc i mt gc no gi l
. Cht lm quay
mt phng phn cc theo cng chiu kim ng h gi l cht hu tuyn
(k hiu +), cht lm quay mt phng phn cc ngc chiu kim ng
h c gi l cht t tuyn (k hiu -).
0
sng n s
ca n natri) qua lp cht lng hay dung dch ca cht xc nh c b
dy l 1dm.
99
20
D ca mt cht rn l gc quay cc o
c khi cho chm tia sng D truyn qua lp dung dch c nng 1%
(KL/ ) v c b dy 1dm 200C.
to
chm sng chiu vo bn phn cc P to ra nh sng phn cc qua
lng knh thch anh Q i vo cht quang hot ng o C lm quay mt
phng phn cc, chiu ti bn phn tch A (A phi quay i mt gc ng
bng gc ngc vi gc m cht quang hot C lm quay i nh b
phn lm quay th trng quan st li ging nh ban u khi cha
t cht quang hot vo). c m A phi quay chnh l gc quay cc
ca cht quang hot.
1
+ nh gc quay cc ring:
100
rong :
l: chiu di ng o (dm).
d: t trng ca cht lng.
C: nng phn trm ca cht th rn trong dung dch.
Cn c vo gc quay cc o c, c th tnh nng phn trm
ca cht th trong dung dch:
101
4.2.2. Cch xc nh
cht ht m thch hp, hoc sy kh 2 gi 100 105oC.
qun xung mt phng cng c mt lp ch phm cao 4 6mm.
ng mao qun trong bnh ht m trc khi tin hnh o.
102
rong :
:
103
5. ng
6. i
7. B
104
5.3. Cch th
5.3.1. Chun b
- Cho mt th tch thch hp mi trng th (thng l nc) vo
cc.
- Vn hnh my iu nhit nhit ca mi trng th t 370C
0,50C.
- Cho vo mi ng th mt vin nn hoc mt vin nang ri y a
cht do vo tng ng.
5.3.2. Vn hnh thit b
hng gi ng ng th thit b vo trong cc ng cht lng v vn
hnh thit b theo thi gian quy nh.
5.3.3. nh gi kt qu
- Sau thi gian quy nh hoc khi thy cc vin r ht, ly gi
ng th ra khi cc cht lng.
- Mu th c coi l t yu cu v r khi khng cn cn, tr
nhng mnh v nang hoc v bao khng tan ca vin nn, cn li trn
mt li ca thit b th hoc dnh vo b mt di ca a y. u
cn cn th n ch l mt khi mm, khng c c nhn kh rn s thy
c.
Kt qu:
+
u c 6 vin u r ht: Mu th t yu cu v r.
105
= 6,8;
u c 6 vin u r ht: Mu th t yu cu v r.
106
- h trn 6 vin.
- Mu th c coi l t yu cu v r khi khng cn cn, tr
nhng mnh v bao khng tan ca ch phm cn li trn mt li ca
thit b th hoc dnh vo b mt di ca a y. u cn cn th n
ch l mt khi mm, khng c c nhn kh rn s thy c.
- Kt qu:
+ Sau 120 pht trong mi trng acid hydrocloric 0,1M: t c cc
vin th phi cn nguyn vn, khng th hin s gii phng hot cht.
+ Sau ti a 60 pht trong mi trng m phosphat: Quan st bng
mt nu thy cc vin th r ht th ghi thi gian. t c cc vin th
phi r ht.
+ u cn di 2 vin khng t yu cu: h li trn 12 vin na.
Ch phm t yu cu v r khi 16 trong s 18 vin th t r
theo quy nh.
6. PHP TH HO TAN CA VIN NN V VIN NANG
6.1. Khi nim
ho tan ca mt ch phm l t l hot cht c gii phng ra
khi dng thuc theo thi gian vi cc iu kin quy nh trong tng
chuyn lun.
Vi mi ch phm c cc quy nh c th v thit b th, mi trng
ho tan, thi gian th nghim v phn trm hot cht c gii phng
(Ch s Q).
6.2. Thit b
107
108
0,5 C.
6.2.2. Thit b kiu cnh khuy
hit b ny ging nh thit b gi quay m t trn, ch khc l gi
c thay bng cnh khuy D (hnh 15C v 15D). Cnh khuy c lp
t sao cho i qua tm ca trc v cnh di ca n ngang bng vi
mt y ca trc. rc cnh khuy c lp t v tr sao cho khng
lch qu 2mm so vi trc ca bnh v cnh y ca cnh khuy cch
mt y trong ca bnh t 23 - 27mm. hit b c vn hnh sao cho
cnh khuy quay trn mt cch nh nhng v khng c rung ng r
6.3. Cch th
6.3.1. Chun b mi trng ho tan
Mi trng ho tan c ch dn trong tng chuyn lun ring. u
l dung dch m th p phi iu chnh sai khc khng qu 0,05 n
Cho mt th tch quy nh mi trng ho tan ui kh vo bnh
(th tch quy nh 1%). Lm m mi trng ho tan n nhit 37
0,5o
6.3.2. Cho vin vo thit b th
u khng c ch dn g khc th th ng thi trn 6 vin, cho mi
- Khi dng thit b gi quay: cho vin nn hay vin nang vo trong gi
- Khi dng thit b kiu cnh khuy: cho vin nn hay vin nang chm
xung y bnh trc khi cho cnh khuy quay; c th dng mt dy
xon bng kim loi hay thu tinh gi cho vin thuc nm ngang di
y bnh. Cn loi tr bt khng kh khi b mt vin.
6.3.3. Vn hnh thit b
Vn hnh thit b ngay tc quay c ch dn trong chuyn lun
ring.
6.3.4. Ly mu lc mu
109
Yu cu kt qu
(Phn trm hot cht ho
tan)
- Khng t. Lm ln 2.
2
- t: Mu th t yu cu
v ho tan. Dng th
nghim.
- Khng t. Lm ln 3.
12
110
- t: Mu th t yu cu
v ho tan.
vin < Q - 15% v khng
c vin no < Q - 25%
- Khng t: Mu th khng
t yu cu v ho tan.
6,8. h trong
+ rong mi trng m p
6,
Yu cu kt qu
(Phn trm hot cht
ho tan)
Khng c vin no vt
10% so vi hm lng
ghi trn nhn.
12
6.5. V d
111
i quay.
ml nc.
60 pht.
Ly mu v x l mu: Lc dung dch sau khi ho tan. Pha long
dch lc vi dung dch m phosphat p 7,2 c dung dch
ibuprofen c nng thch hp.
o hp th ca dung dch thu c bc sng 221nm trong
cuvet thch anh c chiu dy 1cm vi mu trng l dung dch m
phosphat pH 7,2.
nh hm lng ibuprofen theo A (1%, 1cm) l 449 bc sng
221nm.
Yu cu: Khng c t hn 85% lng ibuprofen (C 13H18O2) ghi
trn nhn c ho tan trong 60 pht.
T LNG GI V BI TP
112
B. 5
C. 6
113
D. 7
B. 15 pht
C. 16 pht
D. 17 pht
B. 30 pht
C. 35 pht
D. 25 pht
B. 0,10 n v
C. 0,05 n v
D. 0,07 n v
B. 3%
C. 4%
D. 2%
114
Bi 8
KIM NGHIM THUC BT, THUC CM
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh
gi cht lng thuc bt, thuc cm.
- Gii thch v nh gi c kt qu kim nghim i vi mt mu
kim nghim thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc bt.
115
116
Dng 1 ry
Dng 2 ry
- Bt th
1400
1400/355
- Bt na th
710
710/250
- Bt na mn
355
355/180
- Bt mn
180
180/125
- Bt rt mn
125
125/90
V d:
kim tra mn ca bt st trng A c yu cu l bt mn, dng 2
ry s 180 v 125. gi ta lm nh sau: ry s 180 ln trn ry s
125, cho 10,0027g ch phm ln ry s 180 v tin hnh ry. Lng bt
qua ry s 180 l 9,6703g; ton b bt qua ry s 180 c ry qua ry
s 125 v lng bt qua ry s 125 l 3,5935 g.
Lng ch phm (%) qua ry s cao hn l:
117
10
Trn 6,00g
118
i 100mg
15
rn 100mg ti 1g
10
rn 1g n 5g
Trn 5g
119
mc 3, bi 13.
1.3.3. Thuc bt pha tim
thuc bt v yu cu i vi thuc tim, thuc tim truyn dng bt nh:
v khun, cht gy st,...
120
121
B. 355
C. 710
D.
B. 355
C. 710
D.
b) Bt na th
A. 180
1400
122
c) Bt na mn
A. 1400
355
B. 125
C. 710
D.
B. 710/250
C. 180/125
D.
B. 710/250
C. 180/125
D.
b) Bt rt mn
A. 125/90
355/180
B. 3%
C. 7%
D.
B. 7%
C. 3%
D.
B. 12%
C. 8%
D.
B. 6%
C. 8%
D.
b) Biosubtin 1g
A. 10%
5%
c) Augmentin 0,5g
A. 10%
5%
d) Magnesi sulfat 5g
A. 10%
5%
B. 12%
123
C. 8%
D.
B. 12%
C. 8%
D.
4,9674g;
5,0923g;
4,8845 g.
Bi 9
KIM NGHIM THUC VIN NANG,VIN NN
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh
gi cht lng thuc vin nang, vin nn.
- Gii thch v nh gi c kt qu kim nghim i vi mt mu
kim nghim thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc vin
nang, vin nn.
124
7,5
1.2.5. ho tan
vin nang"
1.2.6. nh tnh
125
i 50mg
10
rn 50mg ti 100mg
7,5
Trn 100mg
126
V d:
Yu cu
Phng php th
1. nh cht
Cm quan.
2. nh tnh
Amoxicilin.
3. ng
u khi
lng
4. c
Khng qu 14,5%.
5. ho tan
Khng c t hn 70,0%
amoxicilin C16H19N3O5S so vi
lng ghi trn nhn c ho
tan sau 60 pht.
6. nh lng
m lng amoxicilin
C16H19N3O5S phi t 92,5 n
110,0% so vi lng ghi trn
nhn (tnh theo loi khan).
127
o tan 0,2g
- Dung dch iod 0,01 : o tan 13g iod tinh th vo mt dung dch
cha 20g kali iodid trong 50 ml nc. Pha long vi nc va 1 lt.
Pha long 10 ml dung dch ny thnh 100 ml bng nc.
- Dung dch natri thiosulfat 0,01 : o tan 26g natri thiosulfat v 0,1g
natri carbonat trong nc khng c carbon dioxyd va 1 lt. Pha
long vi nc va 1 lt. Pha long 10 ml dung dch ny thnh 100 ml
bng nc.
- Dung dch amoxicilin chun 1mg/ ml (CC): Cn chnh xc mt lng
amoxicilin trihydrat chun tng ng khong 100mg amoxicilin v cho
vo bnh nh mc 100 ml. o tan v thm nc va 100 ml.
c) Phng php th
nh tnh:
128
ml nc.
pht.
ml dch lc
u, pha long nu cn. o hp th bc sng 272nm (Ph lc 3.1
dung dch amoxicilin trihydrat chun trong nc c nng tng
ng.
Yu cu: Khng c t hn 70,0% amoxicilin C16H19N3O5S so vi
lng ghi trn nhn c ho tan sau 60 pht.
nh lng:
Amoxicilin trong ch phm c nh lng bng phng php o
iod, nhit 25 20C. Cch tin hnh nh sau:
- Dung dch th: Cn 20 nang, tnh khi lng trung bnh thuc trong
nang mTB (mg), nghin mn. Cn chnh xc mt lng bt thuc mT (mg)
tng ng vi khong 100mg amoxicilin, ho tan trong nc va 100
ml. Lc k, lc, b khong 20 ml dch lc u. Ly chnh xc 2,00 ml
dung dch th cho vo bnh nn nt mi c dung tch 100 ml, thm 2,0 ml
dung dch natri hydroxyd 1 , lc u, yn 15 pht. hm 2,4 ml dung
dch acid hydrocloric 1 v 10,0 ml dung dch iod 0,01 , y ngay nt
129
bnh. yn 15 pht, chun iod tha bng dung dch natri thiosulfat
0,01 n khi dung dch c mu vng. hm 2 git ch th h tinh bt v
chun tip n khi mt mu. hi vT ml.
Ly chnh xc 2,00 ml dung dch th cho vo bnh nn nt mi khc
c dung tch 100 ml, thm 0,12 ml dung dch acid hydrocloric 1 v 10,0
ml dung dch iod 0,01 . Chun ngay bng dung dch natri thiosulfat
0,01 n khi dung dch c mu vng. hm 2 git ch th h tinh bt v
chun tip n khi mt mu. hi VT ml.
- Dung dch chun: Cn chnh xc Ag amoxicilin trihydrat chun
tng ng khong 100mg amoxicilin ho tan trong nc va 100 ml.
2,00 ml,... h tch dung dch natri thiosulfat 0,01
l vC ml v mu trng l VC ml.
130
2.2.2. r
u khng c quy nh ring th tin hnh th v nh gi theo
"Php th r vin nn v vin nang" mc 5, bi 7.
Vin khng cn th r khi php th ho tan c thc hin.
2.2.3. ng u khi lng
Cn chnh xc 20 vin bt k v xc nh khi lng trung bnh ca
vin. Cn ring khi lng tng vin v so snh vi khi lng trung
bnh, tnh lch theo t l phn trm ca khi lng trung bnh, t
tnh ra khong gii hn ca gi tr trung bnh. Khng c qu 2 vin c
khi lng chnh lch qu khong gii hn ca khi lng trung bnh v
khng c c vin no c chnh lch qu gp i lch tnh theo t
l phn trm, theo bng 14.
Bng 14. Gii hn cho php chnh lch khi lng i vi vin nn
Khi lng trung bnh vin
i 80mg
10
rn 80mg n 250mg
7,5
Trn 250mg
109,6mg
118,0mg
116,2mg
107,8mg
114,5mg
116,9mg
120,3mg
122,3mg
119,4mg
112,6mg
109,2mg
111,9mg
117,2mg
115,3mg
113,9mg
120,8mg
116,1mg
118,3mg
131
132
133
Yu cu
Phng php th
1. nh cht
Vin mu trng.
Cm quan.
2. nh tnh
Acid acetylsalicylic.
3. ng
u khi
lng
4. ho tan
5. ii hn
acid salicylic
t do
Khng c qu 0,3%.
6. nh lng
m lng ca acid
acetylsalicylic (C9H8O4) t 95,0
n 105,0% so vi lng ghi
134
trn nhn.
b) Thuc th (theo DVN III)
Cch pha cc dung dch sau c tin hnh nh ch dn phn
thuc th bi 4 v Ph lc 2.8 DV
.
- Dung dch natri hydroxyd 10%.
- Dung dch acid sulfuric 10%.
- Dung dch st ( ) clorid 0,5%.
- Natri acetat.
- Acid acetic bng.
- Ethanol 96%.
- Dung dch phn st amoni 0,2%.
- Dung dch chun natri hydroxyd 0,5
- Dung dch chun acid hydrocloric 0,5
.
.
135
, tng ng vi 45,04mg
T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca vin
nang?
136
B. 6%
C. 5%
D. 7,5%
B. 7,5%
C. 5%
D. 6%
B. 12%
C. 5%
D. 8%
B. 5%
C. 7,5%
D. 10%
B. 12%
C. 11%
D. 8%
C. 7,5%
D. 5%
C. 7,5%
D. 5%
B. 10%
B. 6%
137
Bi 10
KIM NGHIM CC DNG THUC LNG
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh
gi cht lng thuc tim, thuc nh mt, xir thuc.
- Gii thch v nh gi c kt qu kim nghim i vi mt mu
kim nghim thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc tim,
thuc nh mt, xir thuc.
138
1.2.2. trong
- Dung dch tim khi kim tra bng mt thng iu kin quy
nh phi trong v hu nh khng c tp c hc.
139
bng my o p .
1.2.5. v khun
mc 3,
bi 13.
1.2.6. Ni c t vi khun
u c quy
nh trong chuyn lun ring. h theo Ph lc 10.3 - DV
.
khi c quy nh khc.
1.2.7. Cht gy st
140
nh i vi:
+ huc tim ng liu n l c th tch t 15 ml tr ln v khng
c quy nh php th ni c t.
+ huc tim ng liu n l c th tch nh hn 15 ml nhng trn
nhn c ghi "khng c cht gy st" v khng c quy nh php th ni
c t.
mc 4, bi
13.
1.2.8. Th tch (i vi thuc tim dng lng)
Cch th: huc tim c thng bng ti nhit phng v phi
c phn tn ng u trc khi th.
a) i vi thuc tim n liu
i vi thuc tim c th tch nh hn hoc bng 5 ml:
+ Ly 6 ng thuc, trng bm tim bng 1 ng, th trn 5 ng.
+ Kim tra bng cm quan 5 ng thuc, thy cc ng th cha th
tch ngang nhau.
+ Dng bm tim kh sch c dung tch khng ln hn 2,5 ln so vi
th tch cn o, c gn kim tim thch hp. Ly thuc sao cho trong bm
tim khng c bt kh v trong kim tim vn cha y thuc tim. Ln
lt ly thuc ca tng ng tim theo cch .
ml:
+ Ly 4 ng thuc, trng bm tim bng 1 ng, th trn 3 ng.
+ Cch tin hnh nh i vi thuc tim c th tch khng ln hn 5
ml.
b) i vi thuc tim nhiu liu trong 1 l v thuc tim truyn tnh
mch th th tch phi ln hn so vi s liu quy nh c ly ra.
bng bm tim chun hoc ng ong chun sch, kh, c chnh xc
ph hp ( h tch khng ln hn 2,5 ln th tch cn xc nh).
gii hn cho
php theo bng 15.
Bng 15. Gii hn cho php v th tch i vi thuc tim
141
i 50 ml
+ 10
Trn 50 ml
+5
142
Dng bt
10
1.3. V d
Kim nghim thuc tim Pyridoxin hydroclorid (Thuc tim vitamin
B6), ng ng 1 ml theo DVN III:
pha thuc tim.
uc tim"
8H11NO3.
Cl t 95,0 n
Yu cu
Phng php th
1. nh cht
Cm quan.
2. pH
2,5 3,5.
o bng my o
143
pH.
3. v
khun
4. h tch
5. nh tnh
Pyridoxin.
Clorid.
6. nh
lng
c) Phng php th
Tnh cht:
Dung dch trong, khng mu.
nh tnh:
0,1g pyridoxin hydroclorid, ho vi nc va 10 ml.
144
145
2.2.2. trong
huc nh mt dng dung dch phi trong, khng c cc tiu phn
khi quan st bng mt thng v t yu cu v trong theo tng
chuyn lun.
huc nh mt dng hn dch c th lng ng, nhng khi lc phi
phn tn d dng v ng nht trong ton khi.
Cch xc nh: trong c xc nh bng cch so snh cc dung
dch vi cc hn dch mu i chiu. h theo Ph lc 5.12 - DV
III.
2.2.3. Th tch
h tch thuc nh mt phi nm trong gii hn 100 - 110% so vi
th tch ghi trn nhn i vi mi th tch ng gi.
Cch th: Ly 5 n v ng gi bt k. Xc nh th tch ca tng
n v bng bm tim chun hoc ng ong chun sch, kh, c
chnh xc ph hp ( h tch khng ln hn 2,5 ln th tch cn xc
nh).
h tch mi n v phi nm trong gii hn cho php.
u c mt n v khng t th phi kim tra li ln th hai ging
nh ln u. u ln th hai c qu mt n v khng t th l thuc
khng t yu cu.
2.2.4. pH
p
o bng my o p .
2.2.5. v khun
huc nh mt phi v khun.
Cch th: u khng c quy nh ring th tin hnh th v nh gi
theo "Th v trng" mc 3, bi 13.
2.2.6. Gii hn cc tiu phn
h nghim ny ch yu cu i vi thuc nh mt dng hn dch.
Cho mt th tch ch phm thch hp vo cc o hay vt knh ca
g
pha rn.
146
Kt qu:
2.2.7. nh tnh
in hnh nh tnh theo cc phng php c quy nh trong tiu
chun, thuc nh mt phi cho cc phn ng ca cc hot cht c trong
2.2.8. nh lng
Ly thuc ca 5 n v ng gi nh nht bt k, trn u. in hnh
nh lng theo cc phng php c quy nh trong tiu chun, hm
lng ca tng hot cht trong ch phm phi nm trong gii hn cho
2.3. V d
Kim nghim thuc nh mt km sulfat ng l 10 ml DVN III:
L dung dch v khun ca km sulfat trong nc ct c lm
ng trng bng cch cho thm cc mui thch hp.
cc yu cu ca chuyn lun ring.
m lng ca km sulfat ZnS
4.7H2
t 95,0 n 105,0% so vi
Yu cu
Phng php th
1. nh cht
Cm quan.
2. pH
4,5 - 5,5.
o bng my o p .
3. v
khun
4. h tch
10 11 ml.
5. nh tnh
on km v sulfat.
147
6. nh lng
m lng ca km sulfat
ZnSO4.7H2 t 95,0 n
105,0% so vi lng ghi
trn nhn.
10.
n hp ch th en eriocrom .
c) Phng php th
Tnh cht:
Dung dch trong sut, khng mu.
nh tnh:
Dung dch ch phm cho cc phn ng ca cc ion km v sulfat
Ly 5 ml dung dch ch phm cho vo ng nghim, thm 1 ml dung
dch acid hydrocloric 2M ( ) v 1 ml dung dch bari clorid 5% ( ), s c
ta trng c to thnh.
Ly 2 ml dung dch ch phm cho vo ng nghim, thm 1 ml dung
dch amoniac 6M ( ) to thnh ta trng, ta ny tan khi thm 1 ml
dung dch amoni clorid ( ). hm 1 ml dung dch dinatri hydrophosphat
( ) s c ta kt tinh mu trng.
pH: 4,5 n 5,5 (Ph lc 5.9 DV
v khun:
148
).
nh lng:
Ly chnh xc mt th tch thuc nh mt tng ng vi khong
25mg km sulfat, thm 50 ml nc v 10 ml dung dch m amoniac p
10,0. Chun bng dung dch dinatri dihydro ethylendiamin tetraacetat
0,01 M, dng hn hp en eriocrom lm ch th (C ).
(1 ml dung dch dinatri dihydro ethylendiamin tetraacetat 0,01 M
tng ng vi 2,875mg ZnS 4.7H2O).
3. KIM NGHIM XIR THUC
3.1. Khi nim
Xir l dung dch m c ca ng trng trong nc, c cha cc
dc cht hoc cc dch chit t dc liu v cc cht thm.
3.2. Yu cu cht lng v phng php th
3.2.1. Tnh cht
Ch phm phi trong, khng c c mi l, bt kh hoc bin cht
trong qu trnh bo qun.
Cch th: h bng cm quan.
3.2.2. trong
Xir thuc phi t yu cu v trong theo tng chuyn lun.
Cch xc nh: trong c xc nh bng cch so snh cc dung
dch vi cc hn dch mu i chiu. h theo Ph lc 5.12 - DV
III.
3.2.3. pH
p
bng my o p .
3.2.4. T trng
trng phi nm trong gii hn quy nh.
in hnh o t trng bng t trng k, picnomet, cn thu tnh Morh
Westphal nh ch dn mc 1, bi 7.
3.2.5. Th tch
149
i 100 ml
+ 10
rn 100 ml ti 250 ml
+8
Trn 250 ml
+6
huc c A, B
huc thng
10
150
phn 1.2.5, bi
8.
T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca thuc
tim.
2. rnh by cch tin hnh v nh gi kt qu th ng u th
tch ca thuc tim thiamin hydroclorid ng ng 1 ml.
3. rnh by cch tin hnh v nh gi kt qu th ng u khi
lng ca thuc tim benzylpenicilin ng l 1g.
4. in hnh nh lng vitamin B12 trong ng tim vitamin B12 0,5mg/
ml nh sau: Pha long 2,00 ml ch phm trong va 50,0 ml vi
nc. Mt quang ca dung dch ny 361nm trong cc o dy
1cm, dng nc lm mu trng l 0,427.
nh hm lng vitamin B12 trong ch phm. Ch phm c t yu
cu v hm lng khng? Bit vitamin B12 c A (1%, 1cm) bc
sng 361nm l 207.
5. rnh by tiu chun v k thut kim nghim chung ca thuc nh
mt.
6. rnh by phng php tin hnh v tnh kt qu nh lng
cloramphenicol trong thuc nh mt cloramphenicol 0,4%.
7. gi ta tin hnh nh lng natri clorid trong thuc nh mt natri
clorid 0,9% nh sau: Ly chnh xc 10 ml dung dch ch phm cho
vo bnh nn 100 ml, thm 5 git dung dch kali cromat 5%. nh
lng bng dung dch bc nitrat 0,1 c K = 0,9965 ht 15,02 ml.
nh hm lng natri clorid trong ch phm. Ch phm c t yu
cu v hm lng khng? Bit 1 ml dung dch bc nitrat 0,1
tng ng vi 5,844mg aCl.
8. rnh by tiu chun v k thut kim nghim ca xir thuc.
9. gi ta tin hnh nh lng paracetamol trong xir h st tr em
cha 15% paracetamol nh sau: Ly chnh xc 1 ml xir cho vo
bnh nh mc 200 ml, pha long vi dung mi va ti vch.
Lc u, lc (nu cn). Pha long 1,00 ml dch lc thnh 100,0 ml
151
B. 6%
C. 7%
D. 5%
B. +7,5%
C. +5%
D. +10%
B. +5%
C. +7,5%
D. +8%
B. +5%
C. +7,5%
D. +8%
B. +11%
C. +7,5%
D. +10%
c) huc nh mt nemydexan ng l 5 ml
A. +10%
B. +15%
C. +7,5%
D. +8%
B. 2,5%
C. 5%
D.
B. 12%
152
C. 11%
D. 8%
Bi 11
KIM NGHIM THUC M, THUC KEM
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh
gi cht lng thuc m, thuc m tra mt, thuc kem.
- Gii thch v nh gi c kt qu kim nghim i vi mt mu
kim nghim thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc m.
153
Bng 19. Gii hn cho php chnh lch khi lng i vi thuc
m
Khi lng ghi trn nhn
Di 10,0 g
15
10,0 - 20,0 g
10
Trn 50,0 g
1.2.3. ng nht
Cc tiu phn phi phn tn ng u.
Cch th: ly 4 n v ng gi, mi n v khong 0,02 -0,03g, tri
ch phm ln 4 tiu bn, bn trn t mt phin knh. y mi phin
knh bng mt phin knh khc v p mnh cho n khi to thnh mt
vt c ng knh khong 2cm. Quan st vt thu c bng mt
thng, 3 trong 4 tiu bn khng c nhn thy cc tiu phn. u c
cc tiu phn nhn thy trong phn ln s cc vt th phi lm li vi 8
n v ng gi. rong s cc tiu bn ny, cc tiu phn cho php nhn
thy khng c vt qu 2 tiu bn.
1.2.4. nh tnh
Tin hnh nh tnh theo cc phng php c quy nh trong tiu
chun, thuc m phi cho cc phn ng ca cc hot cht c trong ch
1.2.5. nh lng
Cn thuc trong 5 n v ng gi nh nht, tnh khi lng trung
bnh, trn ng nht. Cn mt lng ch phm nh ch dn trong
chuyn lun, tin hnh nh lng. m lng hot cht phi nm trong
Bng 20. Gii hn cho php v hm lng i vi thuc m
Nng hm lng ghi trn
nhn
i 200mg
Trn 200mg - 1g
10
154
Trn 1g - 5g
7,5
Trn 5g
155
t 9,0 n 11,0%.
Yu cu
Phng php th
1. nh cht
Cm quan.
2. ng
u khi
lng
15g 10%.
3. ng
nht
4. nh tnh
Acid boric.
5. nh lng
b) Thuc th
Cch pha cc dung dch sau c tin hnh nh ch dn phn
huc th, bi 4, Ph lc 2.8 - DV
.
- Ethanol.
- Dung dch acid sulfuric m c.
- Dung dch chun natri hydroxyd 0,1
156
nh lng:
Cn chnh xc khong 1g ch phm cho vo cc c m, thm 20 ml
nc v 20 ml phenolphtalein. un cch thu (C ) cho tan. Lc u.
Chun bng dung dch natri hydroxyd 0,1 n khi xut hin mu
hng bn vng (ch th phenolphtalein).
(1 ml dung dch natri hydroxyd 0,1
H3BO3).
tng ng vi 6,183mg
T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca thuc
m.
2. iu chun v k thut kim nghim ca thuc m tra mt c g
khc so vi thuc m ni chung? y trnh by nhng im khc
nhau .
3. rnh by cch tin hnh v nh gi kt qu th ng u
khi lng ca kem ngh ng gi 5g trong 1 tuyp.
Chn cu tr li ng cho cc cu hi t 4 n 6 bng cch khoanh
trn ch ci u cu c chn:
4. Quy nh gii hn cho php v chnh lch khi lng ca thuc
m, thuc kem nh sau:
a) huc m tra mt clorocid
A. 10%
B. 15%
ng gi 4g
C. 12,5%
157
D. 20%
A. 5%
B. 7,5%
C. 8%
D. 6%
C. 15%
D. 8%
B. 12%
B. 7,5%
C. 15%
D. 10%
B. 12%
C. 11%
D. 8%
B. 10%
C. 7,5%
D. 5%
B. 6%
C. 5%
D.
ii hn nhim khun.
158
Bi 12
KIM NGHIM THUC NG DC
MC TIU
- Trnh by c cc yu cu k thut v phng php th nh
gi cht lng thuc hon, ru thuc, cao thuc.
- nh gi c kt qu kim nghim i vi mt mu kim nghim
thnh phm c th ca cc dng bo ch trn.
- Trnh by c v d v kim nghim cc dng bo ch thuc hon,
ru thuc, cao thuc.
159
Phng php 2
Phng php 3
KLTB*
KLTB*
KLTB* ca 1
% chnh
% chnh
160
ca 1
hon
lch
ca 1
phn
lch
n v ng gi
chnh
lch
0,05g
n 1,5g
12%
0,05g
n 0,1g
12%
0,5g tr
xung
12%
rn 0,5g n
1g
11%
Trn 1,5g
n 5g
10%
Trn 5g
n 9g
7%
Trn 9g
5%
Trn 0,1g
n 1g
10%
Trn 1g
7%
rn 1g n 2g
10%
rn 2g n 3g
8%
rn 3g n 6g
6%
rn 6g n 9g
5%
Trn 9g
4%
161
12% nc.
9% nc.
1.4. V d
Kim nghim Hon lc v (hon cng, ng gi 25g) - DVN III:
cc yu cu ca chuyn lun ring.
oi sn
80g
hc a
160g
n b
60g
rch t
60g
Phc linh
60g
Sn th
80g
Mt ong
1000g
Yu cu
Phng php th
1. Tnh cht
Cm quan.
2. m
Khng c qu 9%.
162
chung.
3. ng u
khi lng
KLTB 10%.
4. r
Khng c qu 1 gi.
5. nh tnh
- Bng ct ko hi nc.
- Sinh a.
6. nhim
khun
t yu cu v gii hn nhim
khun.
b) Phng php th
Tnh cht:
Ch phm l hon hnh cu, mu en nhnh. Mi thm dc liu. V
ngt hi chua.
nh tnh:
- Ct ko bng hi nc 10g hon v hng ly 20 ml dch ct, ly 2
ml dch ct, thm 0,5 ml acid benzosulfonic diazo ho, 1 - 2 git natri
carbonat ( ) xut hin dn dn mu da cam.
- nh tnh hc a:
+
+ Bn mng: Silicagel
163
164
Hy thim
1000g
50g
Ethanol 90%
235 ml
ng trng
130g
1000 ml
Yu cu
Phng php th
165
1. nh cht
Cm quan.
2. nh tnh
Hy thim.
3. trong v
ng nht
Cm quan.
4. m lng
ethanol
19% 1%.
5. trng
b) Phng php th
Tnh cht:
Cht lng mu nu en, mi thm hin nin kin, v ngt.
nh tnh:
nh tnh y thim:
C trong 1 gi.
166
trong v ng nht:
Snh, ng nht, khng c c vng mc, b dc liu v vt l.
Hm lng ethanol:
19%
T trng:
20oC: 1,05
trng k).
3. KIM NGHIM RU THUC
3.1. nh ngha
u thuc l dng thuc lng c mi thm v v ngt, iu ch
bng cch ngm dc liu thc vt hoc ng vt ( ch bin) trong
ru hoc ethanol long trong mt thi gian nht nh (tu theo quy nh
ca tng cng thc) ri gn ly ru thuc. m lng ethanol trong
ru thuc khng qu 45%.
3.2. Yu cu k thut v phng php th
3.2.1. Mu sc
167
Cu
tch
g gia
b
Tang
chi
gu
20g
10g
30g
h phc linh
10g
uyt gic
10g
c on
20g
Hy thim
30g
ng
trng
168
130g
tt
10g
th
40g
K huyt
ng
40g
Ethanol
ml
130
Thin nin
kin
30g
Hong
tinh
20g
Yu cu
Phng php th
1. nh cht
2. trong
Cm quan.
3. Hm lng
ethanol
19 - 23%
4. trng
5. lng cn
Lp cn khng c qu 0,5
heo chuyn lun
ml.
chung.
b) Phng php th
Tnh cht:
Cht lng trong, mu nu, mi c bit, v ngt cay.
trong:
1.17 - DV
).
Hm lng ethanol:
19 - 23% (Ph lc 6.15 - DV
).
T trng:
200C: t 1,02 t trng k).
169
lng cn:
Lp cn khng c qu 0,5 ml (Ph lc 1.17 - DV
).
T LNG GI V BI TP
1. rnh by tiu chun v k thut kim nghim chung ca thuc
hon.
2. rnh by tiu chun v k thut kim nghim ca cao thuc.
3. Trnh by tiu chun v k thut kim nghim ca ru thuc.
Chn cu tr li ng cho cc cu hi t 4 n 6 bng cch khoanh trn
ch ci u cu c chn:
4. Quy nh gii hn cho php v chnh lch khi lng ca thuc
hon c ung theo s lng vin nh sau:
a) huc i trng hon c khi lng trung bnh 0,1258g
A. 10%
7%
B. 15%
C. 12%
D.
B. 10%
C. 7%
D.
B. 12%
C. 7%
D.
B. 45 pht
C. 90 pht
D. 120
B. 45 pht
C. 60 pht
170
D. 90
A. 105 pht
pht
B. 120 pht
C. 60 pht
D. 90
B. 15%
C. 20%
D. 10%
C. 20%
D. 10%
B. 15%
Bi 13
MT S PHNG PHP SINH HC
TRONG KIM NGHIM THUC
MC TIU
- Trnh by c phng php lm mi trng nui cy vi sinh vt v
nu c cc phng php kh trng.
- Trnh by c mc ch, nguyn tc, phng php th cht gy
st, v khun v gii hn nhim khun ca ch phm bo ch v
nguyn liu lm thuc.
rong Ph lc 10 ca Dc in Vit am c trnh by phng
php kim nghim thuc bng phng php sinh hc. rong khun kh
ca ti liu ny, chng ti trnh by ba php th nh gi cht lng
thuc l th cht gy st, th gii hn nhim khun v th v trng.
1. YU CU C BN CA PHNG KIM NGHIM VI SINH VT
1.1. Quy tc an ton trong phng kim nghim vi sinh vt
Cn b lm vic ti phng kim nghim vi sinh phi c kin thc
v kinh nghim v cng tc kim nghim vi sinh v phi tun theo cc
quy tc an ton trong khi lm vic.
1.1.1. Yu cu v phng kim nghim vi sinh
Din tch lm vic, cc khu vc trong phng c phn chia v b tr
ph hp, khong cch lm vic hp l hn ch ti a s di chuyn
trong phng (lm xo ng khng kh v lm tng nguy c nhim).
thng chiu sng y , c h thng thng kh trnh s ng bi v
171
172
173
174
175
ngi tin hnh th nghim cn mang gng tay hoc st trng tay vi
cn 70o hoc cc dung dch tit khun, ng thi st trng mt bn thao
tc. Sau khi thc hin xong vic cy chng li tin hnh st trng tay,
mt bn tng t nh trn.
t nng u que cy trong ngn la v t
nh phn cn. Cm thng ng que cy ln cho que nng u. M nt
bng v a ngay que cy kh trng vo dng c cha ging. p
u que cy vo thnh ng nghim, bnh cha hoc t nh ln phn
mi trng khng cha vi sinh vt lm ngui que cy trc khi ly vi
sinh vt.
176
15,0g
Pepton u tng
5,0g
NaCl
5,0g
hch
15,0g
c ct
1000 ml
5g
Pepton
10g
NaCl
5g
hch
18g
c ct va
1000 ml
b) Mi trng xc nh gii hn vi nm
Mi trng thch Sabouraud - Khng sinh:
Pepton
10g
Glucose
20g
hch
20g
c ct
1000 ml
177
2.3.2. Chun b mu th
Mu th theo quy nh chung c ly 10g (hoc 10 ml) th
nghim.
2.3.3. m s lng vi sinh vt
ml cht th nng thch hp sao cho
khng qu 300 khun lc vi khun v 100 khun lc vi nm trong 1 ml.
Thm 15 20 ml mi trng thch casein - u tng hoc mi trng
thch thng i vi a xc nh s lng vi khun v 15 20 ml thch
Sabouraud - khng sinh i vi a xc nh s lng vi nm
ngui di 45oC. ui cy 30 350C trong 1 2 ngy i vi a xc
nh s lng vi khun v 25 28oC trong 4 5 ngy i vi a xc
nh s lng vi nm.
V d: Xc nh s lng vi khun hiu kh, vi nm trong 1 ml b ph
ch khi l.
in hnh: Dng cn 70o st trng bn ngoi l. Ly 10 ml ch phm
pha vo 90 ml dung dch aCl 0,9% c nng pha long 10-1.
Pha long tip c nng 10-2. Cho vo mi hp petri 1 ml dung dch
cht th ca mi nng . hm 15 ml dung dch mi trng thch
thng un chy ngui khong 45 oC i vi a xc nh s lng
vi khun, v mi trng Sabouraud khng sinh i vi a xc nh s
lng vi nm. Xoay nh a cht th trn u vo mi trng. Mi
nng lm 2 a th song song. iu kin nui cy nh trn.
trn cc a th.
2.3.4. Tnh kt qu
ng s vi khun hiu kh, vi nm trong 1g (1 ml) c tnh theo
cng thc:
178
Yu cu
Cc ch phm dng ti
ng s vi khun hiu kh khng qu 100
ch nh cha sng ty, trong 1g ( ml).
tn thng v cc mng
nhy (mi, hng, tai, m Mu th phi khng c nm v mc trong
1g ( ml).
o),...
Cc ch phm dng ti
ch cho da nh kem
bi, nc thm, du,
dung dch, bt,...
Cc ch phm dng
ung; qua trc trng;
thm qua da.
Cc ch phm c cha
ng s vi khun hiu kh sng li c
cc nguyn liu c
khng qu 5.104 trong 1g ( ml).
ngun gc thc vt,
m v mc khng qu 500 trong 1g (
ng vt khng th x l
theo quy trnh lm gim ml).
lng vi khun.
3. TH V TRNG
3.1. Mc ch
Mc ch ca th v trng nhm pht hin s c mt ca vi khun, vi
nm trong cc ch phm nh dch tim truyn, mt s loi thuc tim,
thuc tra mt v cc dng c y t (dng c phu thut m theo tiu
chun ring cn phi v trng).
3.2. Nguyn tc
Vi sinh vt c trong ch phm th s pht trin trn cc mi trng
dinh dng thch hp; trong mi trng lng, vi sinh vt lm c mi
trng, to vng trn b mt hoc lng cn y ng nghim; trn mi
trng c vi khun, vi nm mc thnh cc khun lc c trng.
179
3.3. Mi trng
rong nhiu Dc in, pht hin vi khun hiu kh, k kh
thng dng mi trng hioglycolat lng v pht hin vi khun, vi
nm dng mi trng Casein - u tng lng. uy nhin, c th dng
cc mi trng khc cho th nghim, vi iu kin cc mi trng ny
thch hp cho s pht trin ca loi vi sinh vt cn pht hin nh mi
trng canh thang cao tht - pepton pht hin vi khun hiu kh; mi
trng Wilson - Blair pht hin vi khun k kh; mi trng Sabouraud
lng pht hin vi nm.
V d:
- Mi trng Thioglycollat:
Agar
0,75g
Yeast extract
5,0g
Pepton casein
15,0g
Glucose
5,5g
Na thioglycollat
0,5g
NaCl
2,5g
L-Cystine
0,5g
Resazurin
0,001g
c ct
1 lt
17,0g
Pepton u tng
3,0g
NaCl
5,0g
K2HPO4
2,5g
Glucose
2,5g
c ct
1000 ml
180
= 6,9
it trng 121o
3.4. Phng php th
h v trng bng phng php nui cy trc tip c k thut n
gin, nhng kh nng pht hin vi sinh vt gim khi s lng vi sinh vt
c t v phn phi trong mt th tch cht th ln. Phng php ny
khng thc hin c vi cc ch phm c tc dng c ch v cc cht
khng sinh, v khi th nghim cht th c cy trc tip vo cc mi
trng nui cy thch hp cho cc vi khun, vi nm.
3.4.1. Lng mu th dng trong th nghim
Lng mu th cn cy vo cc mi trng tu thuc vo tng loi
mu (bng 23).
Bng 23. Lng mu th dng cho th nghim nui cy trc tip
Lng ch phm
trong mt n v ng
gi
Th tch mi
trng
Cht lng:
h tch V < 1 ml
1 ml
ml
4 ml
ml
20 ml
ml
50 ml
ml
ml
on b mt ng
10 ml
1/2 ng
15 ml
2 ml
20 ml
5 ml
40 ml
10 ml
80 ml
hng 10%
100 ml
on b mt n v ng gi
20 ml
Cht rn:
Khi lng P < 50mg
50mg < P < 200mg
40 ml
100mg
80 ml
181
182
183
184
P N
Bi 1
Bi 4
5. a) A, D
7. 1,0619
185
b) B, C
8. 1,0848
13. a) A: cam; B: vng
6. a) C
b) A: ; B: vng
b) B
Bi 2
c) A: vng; B:
7. a) cao hn
d) A: trng; B:
b) c tnh thc t
14. a) A
c) chnh xc
b) B
8. a) A
c) D
b) D
15. a) A
c) B
b) D
Bi 5
d) D
4. a) pha lng
9. a) B
b) C
b) lc ly tm
c) A
c) dung mi
10. a) C
b) A
14. 0,22V
Bi 3
4.
15. 0,276%
m lng: 0,02756g/l
16.
ml
17. a) A
Kt qu x l thng k:
b) B
= 0,92756 0,000611(g/l)
18. a) B
b) C
c) B
C: t
19. a) A
186
D: nung
b) C
c) B
Bi 7
Bi 10
9. 1,134
4. 0,5157mg/ ml. t
10. 1,458
7. 0,875%. t
11. 19,89
9. t (14,65%)
12. a) C
10. a) C
b) B
b) D
c) C
c) B
13. a) A
11. a) A
b) B
b) D
c) A
12. a) C
Bi 8
3. a) D
b) A
Bi 11
b) C
4. a) B
c) D
b) C
4. a) C
c) A
b) A
d) C
5. a) B
5. a) A
b) B
b) B
c) A
c) D
d) D
6. a) A
6. A
Bi 12
187
b) D
4. a) C
7. t
b) B
Bi 9
c) C
3. a) D
5. a) A
b) C
b) C
c) C
c) B
d) B
6. a) C
4. a) A
b) A
b) B
Bi 13
c) D
11. a) A
5. D, E
b) C
7. Khng t
8. t (99,45%)
188
Ph lc 1
BNG NGUYN T LNG CC NGUYN T
heo ti liu ca Lin on quc t v ho hc thun tu v ng
dng xut bn nm 1989 (Pure App.Chem.1991,63,978.)
Tn nguyn t *
K hiu
Nguyn t s
Nguyn t lng
Argon
Ar
18
39,948
Arsen
As
33
74,9216
Bc (Argentum)
Ag
47
107,8682
Bari
Ba
56
137,327
Beryli
Be
9,0122
Bismuth
Bi
83
208,9804
Bor
10,811
Brom
Br
35
79,904
Cadmi
Cd
48
112,411
Cesi
Cs
55
132,9054
Calci
Ca
20
40,078
Carbon
12,011
Ceri
Ce
58
140,115
Ch (Plumbum)
Pb
82
207,2
Clor
Cl
17
35,4527
Crom
Cr
24
51,9961
Cobalt
Co
27
58,9332
ng (Cuprum)
Cu
29
63,546
Dysprosi
Dy
66
162,50
Erbi
Er
68
167,26
Europi
Eu
63
151,965
Fluor
18,9984
gadolini
gd
64
157,25
189
gali
ga
31
69,723
germani
ge
32
72,61
Hafni
Hf
72
178,49
Heli
He
4,0026
Holmi
Ho
67
163,9303
Hydrogen
1,0079
Indi
In
49
114,82
Iod
53
126,9045
Iridi
Ir
77
192,22
Kali
19
39,0983
Km (Zincum)
Zn
30
65,39
Krypton
Kr
36
83,80
Lanthan
La
57
138,9055
Lithi
Li
6,941
Luteti
Lu
71
174,967
Lu hunh (Sulfur)
16
32,066
Magnesi
Mg
12
24,3050
Mangan
Mn
25
54,9381
Molybden
Mo
42
95,94
Natri
Na
11
22,9898
Neodymi
Nd
60
144,24
Neon
Ne
10
20,1797
Nhm (Aluminium)
Al
13
26,9815
Nickel (Niccolum)
Ni
28
58,6934
Niobi
Nb
41
92,9064
Nitrogen
14,0067
Osmi
Os
76
190,2
190
Oxygen
15,9994
Paladi
Pd
46
106,42
Phosphor
15
30,9738
Platin
Pt
78
195,08
Praseodymi
Pr
59
140,9077
Rheni
Re
75
186,207
Rhodi
Rh
45
102,9055
Rubidi
Rb
37
85,4678
Rutheni
Ru
44
101,07
Samari
Sm
62
150,36
St ( ron)
Fe
26
55,847
Scandi
Sc
21
44,9559
Selen
Se
34
78,96
Silic (Silicium)
Si
14
28,0855
Stibi (Stibium)
Sb
51
121,757
Stronti
Sr
38
87,62
Tantal
Ta
73
180,9479
Techneti
Tc
43
(97)
Telur
Te
52
127,60
Terbi
Tb
65
158,9253
Thali
Tl
81
204,3833
Sn
50
118,70
Thori
Th
90
232,0381
Thuli
Tm
69
168,9342
hu ngn
(Hydrragyrum)
Hg
80
200,59
Titan
Ti
22
47,88
Uran
92
238,0289
hic (Stanium)
191
Vanadi
23
50,9415
Vng (Aurum)
Au
79
196,9665
Wolfram
74
183,85
Xenon
Xe
54
131,29
Yterbi
Yb
70
173,04
Ytri
39
88,9059
Zirconi
Zn
40
91,224
Ph lc 2
CC PHN NG NH TNH MT S ION
Acetat
A. un nng ch phm vi cng mt lng acid oxalic (
c mi acid acetic.
B.
).
i xng ra
Amoni (mui)
A.
B.
Bc (mui)
A.
192
B.
Bari (mui)
A. Ly mt lng dung dch mui bari nh ch dn trong chuyn lun,
thm vi git acid sulfuric long ( ) s xut hin ta trng, ta ny
khng tan trong acid hydrocloric 10% (TT) v acid nitric long (TT).
B. Dng mt dy bch kim hoc a thu tinh ly mt lng cht th t
trn ngn la khng mu, ngn la s nhum thnh mu xanh lc hi
vng, khi nhn qua knh thu tinh mu lc ngn la s c mu xanh.
Benzoat
A. Ly 1 ml dung dch trung tnh 10% ca ch phm, hoc mt lng
ch phm theo ch dn trong chuyn lun, thm 0,5 ml dung dch st
( ) clorid 10% ( ) s xut hin ta vng thm, ta ny tan trong
ether (TT).
B. Ly khong 0,2g ch phm hoc mt lng ch phm theo ch dn
trong chuyn lun, lm m bng 0,2 ml n 0,3 ml acid sulfuric ( )
v un nng nh y ng nghim, s c cc tinh th thng hoa
trng bm thnh trong ca ng.
C.
Bismuth (mui)
A. hm 10 ml acid hydrocloric 10% ( ) vo 0,5g ch phm, hoc dng
10 ml dung dch theo ch dn trong chuyn lun. un si trong 1 pht,
ngui ri lc nu cn. hm 20 ml nc vo 1 ml dung dch thu
c trn, xut hin ta trng hay hi vng, ta ny s chuyn
thnh nu khi thm 0,05 n 0,1 ml dung dch natri sulfid ( ).
B. hm 10 ml dung dch acid nitric 2M ( ) vo 40 n 50mg ch phm,
hoc dng 10 ml ch phm c x l theo ch dn trong chuyn
lun. un si trong 1 pht, ngui ri lc nu cn. hm 2 ml dung
dch thioure 10% ( ) vo 5 ml dch lc thu c trn, xut hin
mu vng da cam hay ta da cam. hm 4 ml dung dch natri fluorid
2,5% ( ), dung dch khng c mt mu trong vng 30 pht.
193
Borat
A.
B.
Calci (mui)
A. Ly khong 20mg ch phm, hoc mt lng ch phm theo ch dn
trong chuyn lun, ho tan trong 5 ml dung dch acid acetic 5 M ( ),
thm 0,5 ml dung dch kali ferocyanid ( ), dung dch vn trong, thm
khong 50mg amoni clorid ( ), to thnh ta kt tinh trng.
B. hm vo dung dch ch phm theo ch dn trong chuyn lun vi git
dung dch amoni oxalat 4% ( ), to thnh ta trng, ta ny t tan
trong acid acetic 6 M ( ), nhng tan trong acid hydrocloric ( ).
Ch (mui)
A.
B.
194
Citrat
A.
B.
Clorid
A.
B.
Iodid
A.
195
Kali (mui)
A.
B.
Km (mui)
o tan 0,1g ch phm trong 5 ml nc, hoc dng 5 ml dung dch
theo ch dn trong chuyn lun. hm 0,2 ml dung dch natri hydroxyd
10 M ( ), to thnh ta trng, ta ny tan khi thm 2 ml natri
hydroxyd 10 M ( ). hm 10 ml dung dch amoni clorid ( ), dung
dch vn trong, thm 0,1 ml dung dch natri sulfid ( ), ta bng trng
c to thnh.
Magnesi (mui)
o tan khong 15mg ch phm trong 2 ml nc, hoc ly 2 ml dung
dch theo ch dn trong chuyn lun. hm 1 ml dung dch amoniac 6
M ( ), to thnh ta trng, ta ny tan khi thm 1 ml dung dch
amoni clorid ( ). hm 1 ml dung dch dinatri hydrophosphat ( ), s
c ta kt tinh trng.
Natri (mui)
A. Dng mt dy bch kim hay a thu tinh, ly mt ht cht th hay
mt git dung dch ch phm, a vo ngn la khng mu, ngn la
s nhum thnh mu vng.
B.
196
B.
Peroxyd
A.
197
A.
B.
St (II) (mui)
o tan mt lng ch phm tng ng vi 10mg st ( ) trong 1 ml
nc, hoc dng 1 ml dung dch theo ch dn trong chuyn lun.
hm 1 ml dung dch kali fericyanid ( ), to ta xanh lam, ta ny
khng tan trong dung dch acid hydrocloric 2 M ( ).
St (III) (mui)
A.
B.
Sulfat
A. Ho tan 45mg ch phm trong 5 ml nc, hoc dng 5 ml dung dch
theo ch dn trong chuyn lun, thm 1 ml dung dch acid hydrocloric
2 M ( ) v 1 ml dung dch bari clorid 5% ( ), s c ta trng c
to thnh.
B. hm 0,1 ml iod 0,1 vo hn dch thu c phn ng trn, hn
dch c mu vng (phn bit vi sulfid v dithionit) nhng mt mu khi
thm tng git dung dch thic ( ) clorid ( ) (phn bit vi iodat).
un si hn hp, khng c to thnh ta c mu (phn bit vi
selenat v tungstat).
Sulfid
198
B.
Ph lc 3
PHN Ng MU CA CC PENICILIN
V CEPHALOSPORIN
A. Cho 2mg ch phm vo mt ng nghim (kch thc 15cm 1,5cm),
lm m vi 0,05 ml nc, thm 2 ml acid sulfuric ( ). Lc u hn
hp v quan st mu ca dung dch. t ng nghim trong cch thu
si trong mt pht v li quan st mu. Mu sc ca dung dch c
quy nh trong bng di y.
B. Lp li cch th nh phn ng A, nhng thay 2 ml acid sulfuric (TT)
bng 2 ml dung dch formaldehyd trong acid sulfuric ( ). Mu sc
ca dung dch c quy nh trong bng di y.
Phn ng mu ca cc penicilin v cephalosporin
Tn mu
Amoxicilin natri
Amoxicilin
Acid
sulfuric
(TT)
Acid
sulfuric
Dung dch
(TT)
formaldehyd trong
sau 1
acid sulfuric (TT)
pht
100oC
Dung dch
formaldehyd
trong acid
sulfuric (TT) sau
1 pht 100oC
u nh khng
mu
Vng sm
u nh khng
Vng sm
199
trihydrat
mu
Ampicilin
u nh khng
mu
Vng sm
Ampicilin natri
u nh khng
mu
Vng sm
Ampicilin
trihydrrat
u nh khng
mu
Vng sm
Benzathin
penicilin
u nh khng
mu
Benzylpenicilin
kali
u nh khng
mu
Benzylpenicilin
natri
u nh khng
mu
Cephalexin
Vng nht
Vng sm
nu
nu
Cloxacilin natri
Vng
Dicloxacilin
natri
Vng
Flucloxacilin
natri
Vng
u
nh
khng
mu
Cephaloridin
Vng
nht
Cephalothin
natri
Vng
ng
(mu
nu
chuyn
nhanh)
Phenoxymethyl
penicilin
u sm
Phenoxymethyl
penicilin kali
u sm
Procain
penicilin
u
nh
khng
mu
u
nh
khng
mu
u nh khng
mu
200
2. rng i hc Y dc thnh ph
kim nghim thuc.
XB Y hc.
201