CNG HO X HI CH NGHA VIT NAM

QCVN 4 - 18 : 2011/BYT




QUY CHUN K THUT QUC GIA

V PH GIA THC PHM NHM CH PHM TINH BT

National technical regulation on Food Additive Modified starches














H NI - 2010
QCVN 4 - 18 : 2011/BYT
2









Li ni u
QCVN 4-18:2011/BYT do Ban son tho quy chun k thut
quc gia v Ph gia thc phm v cht h tr ch bin bin
son, Cc An ton v sinh thc phm trnh duyt v c ban
hnh theo Thng t s 01/2011/TT-BYT ngy 13 thng 01 nm
2011 ca B trng B Y t.



QCVN 4 - 18 : 2011/BYT
3
QUY CHUN K THUT QUC GIA
V PH GIA THC PHM CH PHM TINH BT
National technical regulation on Food Additive Modified starches


I. QUY NH CHUNG

1. Phm vi iu chnh
Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc yu cu
k thut v qun l v cht lng, v sinh an ton i vi cc ch phm tinh bt c s
dng vi mc ch lm ph gia thc phm.

2. i tng p dng
Quy chun ny p dng i vi:
2.1. T chc, c nhn nhp khu, xut khu, sn xut, bun bn v s dng cc
ch phm tinh bt lm ph gia thc phm (sau y gi tt l t chc, c nhn).
2.2. C quan qun l nh nc c lin quan.

3. Gii thch t ng v ch vit tt:
3.1. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food additive specifications; Joint FAO/WHO expert committee on
food additives; Volume 4 - Analytical methods, test procedures and laboratory
solutions used by and referenced in the food additive specifications; FAO, 2006): Cc
yu cu k thut i vi ph gia thc phm, Tp 4 Cc phng php phn tch, quy
trnh th nghim, dung dch th nghim c s dng (hoc tham chiu) trong yu
cu k thut i vi ph gia thc phm; JECFA bin son; FAO ban hnh nm 2006.
3.2. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.3. TS (test solution): Dung dch thuc th.
3.4. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.5. INS (International numbering system): H thng m s quc t v ph gia
thc phm.

QCVN 4 - 18 : 2011/BYT
4
II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi:
- Dextrin, tinh bt rang
- Tinh bt x l bng acid
- Tinh bt x l bng kim
- Tinh bt ty mu
- Tinh bt oxy ho
- Tinh bt x l bng enzym
- Monostarch phosphat
- Distarch phosphat
- Distarch phosphat phosphat ho
- Distarch phosphat acetylat
- Tinh bt acetat
- Distarch adipat acetylat
- Tinh bt hydroxypropyl
- Distarch phosphat hydroxypropyl
- Tinh bt natri octenylsucinat
s dng lm ch phm tinh bt c quy nh ti ph lc ban hnh km theo
Quy chun ny.

2. Cc yu cu k thut quy nh trong Quy chun ny c th theo JECFA
monograph 1 - Vol. 4, ngoi tr mt s php th ring c m t trong ph lc. Cc
phng php th c hng dn trong Quy chun ny khng bt buc phi p
dng, c th s dng cc phng php th khc tng ng.

3. Ly mu theo hng dn ti Thng t 16/2009/TT-BKHCN ngy 02 thng 6
nm 2009 ca B Khoa hc v Cng ngh v hng dn kim tra nh nc v cht
lng hng ha lu thng trn th trng v cc quy nh khc ca php lut c lin
quan.

III. YU CU QUN L

1. Cng b hp quy
1.1. Cc ch phm tinh bt phi c cng b ph hp vi cc quy nh ti
Quy chun ny.
1.2. Phng thc, trnh t, th tc cng b hp quy c thc hin theo Quy
nh v chng nhn hp chun, chng nhn hp quy v cng b hp chun, cng
b hp quy ban hnh km theo Quyt nh s 24/2007/Q-BKHCN ngy 28 thng 9
nm 2007 ca B trng B Khoa hc v Cng ngh v cc quy nh ca php lut.

QCVN 4 - 18 : 2011/BYT
5
2. Kim tra i vi ch phm tinh bt
Vic kim tra cht lng, v sinh an ton i vi cc ch phm tinh bt phi
thc hin theo cc quy nh ca php lut.

IV. TRCH NHIM CA T CHC, C NHN

1. T chc, c nhn phi cng b hp quy ph hp vi cc quy nh k
thut ti Quy chun ny, ng k bn cng b hp quy ti Cc An ton v sinh thc
phm v bo m cht lng, v sinh an ton theo ng ni dung cng b.
2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc ch phm tinh bt sau khi hon tt ng k bn cng b hp quy v bo m cht
lng, v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut.

V. T CHC THC HIN

1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chc
nng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny.
2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhim
kin ngh B Y t sa i, b sung Quy chun ny.
3. Trng hp hng dn ca quc t v phng php th v cc quy nh
ca php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th th
p dng theo vn bn mi.

QCVN 4 - 18 : 2011/BYT
6
Ph lc
YU CU K THUT V PHNG PHP TH
I VI CH PHM TINH BT

1. Tn khc, ch s
Dextrin, tinh bt rang: INS 1400
Tinh bt x l bng acid: INS 1401
Tinh bt x l bng kim: INS 1402
Tinh bt ty mu: INS 1403
Tinh bt oxy ho: INS 1404
Tinh bt x l bng enzym: INS 1405
Monostarch phosphat: INS 1410
Distarch phosphat: INS 1412
Distarch phosphat phosphat ho: INS 1413
Distarch phosphat acetylat: INS 1414
Tinh bt acetat: INS 1420
Distarch adipat acetylat: INS 1422
Tinh bt hydroxypropyl: INS 1440
Distarch phosphat hydroxypropyl: INS 1442
Tinh bt natri octenylsucinat: INS 1450
2. nh ngha Cc tinh bt thc phm c mt hoc vi thuc tnh gc
c thay i do x l ph hp vi GMP, theo mt s quy
trnh nht nh
M s C.A.S.
Tinh bt acetat : 9045-28-7
Distarch adipat acetylat: 68130-14-3
Tinh bt hydroxypropyl: 9049-76-7
Distarch phosphat hydroxypropyl: 53124-00-8
Tinh bt oxy ho acetylat: 68187-08-6
3. Cm quan Hu ht ch phm tinh bt dng bt khng mi, mu trng
hoc trng nht. Tu thuc vo phng php sy, cc bt
ny c th gm cc ht tinh bt nguyn dng gc hoc cc
khi gm nhiu ht (dng qu l, dng mt) hoc nu h
ho trc s gm dng vy, bt v nh hnh hoc dng ht
th.
4. Chc nng Ch phm tinh bt, cht lm dy, cht n nh, cht n,
cht nh ho
5. Yu cu k thut
5.1. nh tnh

tan
Khng tan trong nc lnh (nu khng h ho trc), to
thnh dung dch keo nht in hnh trong nc nng; khng
tan trong ethanol.
Cu trc hin vi
Xem m t trong phn Phng php th
QCVN 4 - 18 : 2011/BYT
7
Nhum mu iod
Phi c phn ng nhum mu iod c trng.
Kh ng
Phi c phn ng kh ng c trng.
Tnh khc bit
Xem phn th i vi dng tinh bt.
Xem m t trong phn Phng php th i vi :
- Tinh bt oxy ho hypoclorid
- Phn ng c trng i vi cc nhm acetyl
- Th dng tnh i vi cc nhm ester
5.2. tinh khit

Lu hunh dioxyd
(SO
2
)
- Khng c qu 50,0 mg/kg i vi ch phm tinh bt t
ng cc
- Khng c qu 10,0 mg/kg i vi cc loi ch phm tinh
bt khc tr khi c ghi r trong bng 1
(xem m t trong phn Phng php th)
Ch
Khng c qu 2,0 mg/kg.
- Th theo JECFA monograph 1 - Vol.4.
- Xc nh bng k thut quang ph hp th nguyn t
thch hp cho hm lng quy nh. La chn c mu th
v phng php chun b mu da trn nguyn tc ca
phng php m t trong JECFA monograph 1 - Vol.4 phn
cc phng php phn tch cng c.
Cc tinh khit b
sung i vi tng loi
ch phm tinh bt ho
hc
- Xem ct 3 bng 1
- Xem m t trong phn Phng php th
6. Phng php th

6.1. nh tnh

Soi knh hin vi
Cc dng ch phm tinh bt khng c h ho trc vn
gi nguyn cu trc ht c th xc nh l tinh bt nh quan
st bng knh hin vi. Hnh dng, kch thc v i khi s
sp xp cc sc hoc ng vn l c trng ca ngun
gc thc vt. Di nh sng phn cc qua lng knh nicol,
gc ct phn cc in c th quan st c.
Nhum mu iod
Cho mt vi git kali tri-iodid 0,1N vo hn dch trong nc
ca mu. Cc tinh bt ny nhum mu iod ging nh
nhum mu vi tinh bt t nhin. Mu c th t mu xanh
m n .
Kh ng
Cho 2,5 g mu trc c ra bng nc vo bnh
chu nhit, thm 10 ml dung dch HCl long 3% v 70 ml
nc, lc u, un vi sinh hn ngc trong 3 gi v lm
ngui. Thm 0,5 ml dung dch thu c vo 5 ml dung dch
kim nng ng (II) tartrat (TS). Kt ta mu thm c
hnh thnh.
QCVN 4 - 18 : 2011/BYT
8
Tnh khc bit
phn bit gia cc loi tinh bt c x l khc nhau,
tin hnh cc php th sau:
- Th i vi tinh bt oxy ho bng hypochlorit (khng th
i vi tinh bt khoai ty oxy ho nh)
Nguyn tc :
V trong thnh phn c cha nhm carboxyl, tinh bt oxy
ho bng hypochlorit c thuc tnh anion. N c th c
nhum bng cc thuc nhum tch in dng nh xanh
methylen.
Cch thc hin:
Gi hn dch gm 50 mg mu th trong 25 ml dung dch
nc thuc nhum 1% trong 5 10 pht v thnh thong
khuy. Sau khi tch dung dch d, tinh bt c ra bng
nc ct. Kim tra bng knh hin vi cho mu r, nu mu
l tinh bt oxy ho hypochlorit. Do vy, php th nyaf cho
php phn bit c tinh bt oxy ha bng hypoclorit vi
tinh bt t nhin hay ch phm tinh bt bng acid c cng
ngun gc thc vt.
- Phn ng c trng ca cc nhm acetyl :
Nguyn tc : Acetat c gii phng nh qu trnh x
phng ho tinh bt acetylat. Sau khi lm giu acetat c
chuyn thnh aceton bng cch gia nhit vi Ca(OH)
2
. Nh
aceton to thnh nhum thnh mu xanh bng ortho-
nitrobenzaldehyd.
Cch tin hnh : To hn dch gm 10 g mu trong 25 ml
nc v thm vo 20 ml dung dch NaOH 0,4N. Sau khi lc
trong 1 gi tinh bt c lc ra v phn dch lc thu c
c trong l 110
0
C. Cn c ho tan trong mt vi git
nc v c chuyn sang ng th. Thm Ca(OH)
2
v gia
nhit ng th. Nu mu l tinh bt acetylat, hi aceton c
hnh thnh. Hi ny to thnh mu xanh trn mnh giy tm
dung dch bo ho o-nitrobenzaldehyd trong NaOH 2N. Mu
xanh rt d nhn thy khi mu vng gc ca cc thuc th
bin mt khi nh 1 git dung dch HCl 10%.
- Th dng tnh i vi cc nhm ester :
Ph hng ngoi tm film mng cho thy mt di hp th
in hnh khong 1.720 cm
-1
biu th s c mt ca cc
nhm ester. Gii hn pht hin l khong 0,5% cc nhm
acetyl, adipyl hoc succinyl trong sn phm.
6.2. tinh khit

QCVN 4 - 18 : 2011/BYT
9
Lu hunh dioxyd
(SO
2
)
Phm vi p dng:
Phng php ny c p dng, vi mt vi thay i nh,
i vi mu cht lng hoc rn thm ch c s c mt ca
cc hp cht cha lu hunh d bay hi khc.
Nguyn tc:
SO
2
c gii phng ra t mu trong mi trng acid un
si v tch kh SO
2
ra bng dng kh CO
2
. Kh tch ra thu
c cho vo dung dch hydrogen peroxid long ni n b
oxy ha thnh H
2
SO
4
v c chun bng dung dch
kim tiu chun. Mt cch khc, H
2
SO
4
c th c nh
lng bng BaSO
4
.
Dng c:
B dng c Monier-Williams nh lng acid sulfur,
c cu to bng cc kt ni thu tinh thon tiu chun, c
th mua c cc ca hng bn dng c thu tinh phc v
nghin cu khoa hc ng tin cy. Tuy nhin, dng c ny
thng c t lp t cc dng c thu tinh th nghim tiu
chun c cc kt ni c np (xem Hnh 1).


Hnh 1
B dng c gm bnh un hai c trn dung tch 1.000 ml ni
vi mt ng kh vo, mt phu nh git dung tch 60 ml c
van kho kch thc l 2 mm, sinh hn ngc nghing
Allihn. Mt ng dn ni vi phn trn cng ca sinh hn ti
y ca bnh nhn hnh nn dung tch 250 ml, bnh ny
dc ni ng Peligot.
Trong qu trnh vn hnh, lng kh CO
2
thot ra c dn
qua bnh by v to thnh bt khi cho qua hn hp phn
ng nng, qut SO
2
qua bnh ngng v vo cc bnh nhn,
ni n c ht nh lng.
Chun b dung dch:

QCVN 4 - 18 : 2011/BYT
10

Dung dch Na
2
CO
3
: Ho tan khong 15 g Na
2
CO
3
hoc 40
g Na
2
CO
3
.10H
2
O trong nc ct v pha ti th tch 100
ml.
Dung dch hydrogen peroxyd 3%: Pha 10 ml hydrogen
peroxyd trung tnh 30% (ho cht tinh khit) vi nc ct
cho n th tch 100 ml.
Cch tin hnh:
Cho CO
2
t my sinh CO
2
hoc bnh kh nn CO
2
qua
dung dch by Na
2
CO
3
loi clor, t cho vo ng dn
kh vo ca bnh un. Cho 15 ml dung dch hydrogen
peroxyd 3% vo bnh nhn v 5 ml vo ng Peligot. Lp
b dng c, cho 300 ml nc ct v 20 ml dung dch HCl
m c vo bnh un bng phu nh git. un si hn
hp trong khong 10 pht c sc kh CO
2
. Cn 100 g mu
chnh xc n tng g v phn tn mu trong khong 300
ml nc ct va un si. Chuyn phn bn nho vo bnh
un bng phu nh git, iu chnh tc mu thm vo
v tc dng kh qua dng c nhm ngn s quay tr li
ca hydrogen peroxyd, k c khng kh, hoc mi kht
ca mu. un si nh hn hp trong 1 gi c sc chm
dng kh CO
2
. Ngng dng nc trong sinh hn trc khi
kt thc chng ct. Khi ng dn ngay bn trn bnh
nhn tr nn nng, tho ng t sinh hn ra ngay lp tc.
Ra cc thnh phn trong ng dn v ng Peligot vo
trong bnh nhn, v chun bng dung dch NaOH 0,1N,
s dng cht ch th xanh bromphenol (xem phn Ch ).
Thc hin th i vi mu trng, kt qu c tnh theo
cng thc sau:
(S B) x 0,0032 x 100
% SO
2
= -------------------------------------
W
Trong :
S: S ml dung dch NaOH 0,1N dng chun mu
th
B: S ml dung dch NaOH 0,1N dng chun mu
trng
W: Khi lng mu th (g)
Ch : Phn tch nh lng bng phng php cn c
th c tin hnh sau khi chun . Acid ho bng HCl,
kt ta bng BaCl
2
, n nh, lc, ra, t chy v cn
tnh theo BaSO
4
.
Bng 1. Cc yu cu k thut v tinh khit b sung i
vi tng loi ch phm tinh bt bin tnh bng ho hc

Loi tinh bt bin
tnh
Tm lc phng
php
Yu cu k thut
i vi sn phm
cui cng

QCVN 4 - 18 : 2011/BYT
11
Dextrin, tinh bt
rang
X l nhit kh vi
acid HCl hoc acid
ortho-H
3
PO
4
pH = 2,5 7,0
Tinh bt x l bng
acid
X l bng acid
HCl hoc ortho-
H
3
PO
4
hoc H
2
SO
4
pH = 4,8 7,0
Tinh bt x l bng
kim
X l bng NaOH
hoc KOH
pH = 5,0 7,5
Tinh bt ty mu X l bng acid
peracetic v hoc
hydrogen peroxid,
hoc natri
hypochlorit, hoc
NaCl, hoc SO
2

hoc cc dng
c cho php
khc ca sulfit,
hoc kali
permanganat hoc
amoni persulfat
Nhm carbonyl
thm vo khng
c qu 0,1%;
Khng c d
lng ho cht;
D lng SO
2

khng c qu
50 mg/kg; D
lng mangan
khng c qu
50 mg/kg.
Tinh bt x l bng
enzym
X l trong dung
dch nc nhit
di im to
keo vi mt hoc
nhiu enzym thu
phn tinh bt dnh
cho thc phm
D lng SO
2

khng c qu
50 mg/kg
Tinh bt oxy ho X l bng natri
hypochlorit
Cc nhm carboxyl
khng c qu
1,1%; D lng
SO
2
khng c
qu 50 mg/kg
Monostarch
phosphat
Ester ho bng
acid ortho-H
3
PO
4
,
hoc natri hoc kali
ortho-phosphat,
hoc natri
tripolyphosphat
Hm lng
phosphat tnh theo
phosphor khng
c qu 0,5% i
vi tinh bt khoai
ty hoc bt m, v
khng c qu
0,4% i vi tinh
bt khc.

QCVN 4 - 18 : 2011/BYT
12
Distarch phosphat Ester ho
bng natri
trimetaphosphat
hoc phospho
oxychlorid
Hm lng
phosphat tnh theo
phosphor khng
c qu 0,5% i
vi tinh bt khoai
ty hoc bt m, v
khng c qu
0,4% i vi tinh
bt khc.
Distarch phosphat
phosphat ho
Kt hp cc x l
i vi Monostarch
phosphat v
Distarch phosphat
Hm lng
phosphat tnh theo
phosphor khng
c qu 0,5% i
vi tinh bt khoai
ty hoc bt m, v
khng c qu
0,4% i vi tinh
bt khc.
Distarch phosphat
acetylat
Ester ho
bng natri
trimetaphosphat
hoc phospho
oxychlorid kt hp
vi ester ho bng
anhydrid acetic
hoc vinyl acetat
Cc nhm acetyl
khng c qu
2,5%; hm lng
phosphat tnh theo
phosphor khng
c qu 0,14%
i vi tinh bt
khoai ty hoc bt
m, v khng c
qu 0,04% i vi
tinh bt khc; v
vinyl acetat khng
c qu 0,1
mg/kg
Tinh bt acetat Ester ho bng
anhydrid acetic
hoc vinyl acetat
Cc nhm acetyl
khng c qu
2,5%
Distarch adipat
acetylat
Ester ho bng
anhydrid acetic v
anhydrid adipic
Cc nhm acetyl
khng c qu
2,5% v cc nhm
adipat khng c
qu 0,135%

QCVN 4 - 18 : 2011/BYT
13
Tinh bt
hydroxypropyl
Ester ho bng
propylen oxyd
Cc nhm
hydroxypropyl
khng c qu
7,0%; propylen
chlorohydrin khng
c qu 1 mg/kg
Distarch phosphat
hydroxypropyl
Ester ho
bng natri
trimetaphosphat
hoc phospho
oxychlorid kt hp
vi ester ho bng
propylen oxyd
Cc nhm
hydroxypropyl
khng c qu
7,0%; propylen
chlorohydrin khng
c qu 1 mg/kg
v d lng
phosphat tnh theo
phosphor khng
c qu 0,14%
i vi tinh bt
khoai ty hoc bt
m, v khng c
qu 0,04% i vi
tinh bt khc
Tinh bt natri
octenylsuccinat
Ester ho bng
anhydrid
octenylsuccinic
Cc nhm
octenylsuccinyl
khng c qu
3%; v d lng
acid
octenylsuccinic
khng c qu
0,3%
Tinh bt oxy ho
acetylat
X l bng natri
hypochlorit sau
ester ho bng
anhydrid acetic
Cc nhm acetyl
khng c qu
2,5% v cc nhm
carboxyl khng
c qu 1,3%
Ch
- Th theo JECFA monograph 1 - Vol.4.
- Xc nh bng k thut quang ph hp th nguyn t
thch hp cho hm lng quy nh. La chn c mu th
v phng php chun b mu da trn nguyn tc ca
phng php m t trong JECFA monograph 1 - Vol.4
phn cc phng php phn tch cng c.
pH - c m t trong Ct 3 ca Bng 1.
- Ha 20 g mu vi 80 ml nc. Khuy lin tc tc
trung bnh trong 5 pht (Trong trng hp mu l tinh bt
keo ha s b, cn 3 g ha vi 97 ml nc).
QCVN 4 - 18 : 2011/BYT
14
Nhm carboxyl c m t trong Ct 3 ca Bng 1.
Nguyn tc:
Tinh bt c cha carboxyl c cn bng vi acid v c
chuyn cc mui carboxyl thnh dng acid. Cc cation
v acid d c loi b bng cch ra vi nc. Mu
ra c ho tan trong nc v c chun bng
dung dch kim chun.
Ch : Cc nhm phosphat t nhin c mt trong tinh bt
khoai ty lm tng chun c tm thy trong phng
php ny ( Xem ghi ch 6 ).
Ho cht, thuc th:
Dung dch HCl 0,1N: Khng cn thit chun ho
Dung dch NaOH 0,1N: c chun ho
Dung dch ch th phenolphthalein 1%
Cch tin hnh:
Nu cn thit, nghin mu hon ton nh my nghin ct
th nghim cho qua ry 20 mesh hoc mn hn, phng
ngn nga bt k s thay i c ngha no v m v
trn u.
Cn chnh xc mt mu cha khng qu 0,25 mili ng
lng carboxyl (Ghi ch 1), v chuyn lng mu vo cc
dung tch 150 ml. Thm vo 25 ml dung dch HCl 0,1N v
thnh thong khuy trn 30 pht. Lc chn khng lp bt
nho qua mt phu thy tinh xp c l xp trung bnhhoc
phu nh, s dng dng nc nh t bnh ra gip
chuyn ton b lng mu. Ra mu bng nc ct
(thng l 300 ml) cho n khi phn dch lc c xc
nh khng c clorid bng php th AgNO
3
(Ghi ch 2).
Chuyn mu kh khong ton lng vo cc dung tch
600 ml cng vi nc ct v chuyn mu thnh bt nho
trong 300 ml nc ct. Gia nhit hn dch mu trong cch
thy si hoc trn cch thy si (Ghi ch 3), khuy lin tc
cho n khi tinh bt ha h v tip tc gia nhit trong 15
pht m bo tinh bt ha h hon ton (Ghi ch 4).
Ly mu ra khi cch thy v chun khi cn nng
bng dung dch NaOH 0,1N im kt thc vi ch th
phenolphthalein. im kt thc cng c th pht hin bng
o in ti pH = 8,3. Xc nh mu trng c tin hnh
ging mu th hiu chnh cc acid t nhin (Ghi ch 5).
Cn cng mt lng tinh bt nh ly chun carboxyl v

QCVN 4 - 18 : 2011/BYT
15
trn ln vi 10 ml nc ct. Khuy u khong 5 pht mi
ln trong 30 pht. Lc chn khng bt nho nh lng
qua mt phu thy tinh xp c l xp trung bnh hoc phu
nh, v ra mu bng 200 ml nc ct. Chuyn, lm h
ha v chun mu bng dung dch NaOH 0,1N ging
nh cch lm i vi mu kh khong.
Kt qu:
(Th tch NaOH chun mu th - mu trng) x 0,0045 x 100
Cc nhm carboxyl (%) = -------------------------------------------------------
Khi lng mu (g)
Ch v phng nga:
Lng mu khng nn vt qu 5,0 g i vi tinh bt oxy
ho trung bnh hoc nh hn 0,15 g i vi tinh bt
thng mi oxy ho cao.
Thm 1 ml dung dch AgNO
3
1% pha trong nc vo 5 ml
dch lc. Xut hin kt ta hoc c trong vng 1 pht nu
c mt ca clorid.
Khng nn gia nhit trn a nng hoc trn n t
Bunsen. S qu nhit hoc qu nng i vi lng mu
nh s lm phn hy mu v kt qu carboxyl cao gi to.
H ha mu trit to iu kin chun nhanh chng
v pht hin im kt thc chnh xc.
Chun mu trng c tin hnh trn mu c
ra bng nc hiu chnh cc thnh phn acid khng
c a vo oxy ho hoc chuyn ho. Cc acid bo
t do kt hp vi amylose trong tinh bt ng thng l
nhng cht c ng gp chnh i vi chun mu
trng.
Hiu chnh hm lng phosphat trong tinh bt khoai ty
(qui i) nn c tin hnh sau khi xc nh hm lng
phospho ca mu th.
Qui i c tnh theo cng thc sau:

Trong : P l hm lng phospho (%)
QCVN 4 - 18 : 2011/BYT
16
Mangan c m t trong Ct 3 Bng 1
Thit b:
Thit b quang ph hp th nguyn t vi n cathod rng
mangan
Chun b dung dch:
Dung dch chun: Chun b dung dch 0,5 mg mangan/lt.
Dung dch mu th: Chuyn 10 g mu vo bnh nh mc
Kohlrausch dung tch 200 ml trc c ra bng
dung dch HCl 0,5N, thm 140 ml dung dch HCl 0,5N v
lc mnh trong 15 pht, thch hp nht dng my lc. Pha
ti th tch 200 ml bng dung dch HCl 0,5N v lc. Li tm
khong 100 ml hn hp trong ng ly tm c thnh dy
hoc l tc 650 xg trong 5 pht v ly dung dch lng
trn b mt. Dung dch ny l dung dch mu th.
Cch tin hnh:
Thc hin theo hng dn ca nh sn xut cho vn hnh
ca thit b quang ph hp th nguyn t v ht nc ct
thng qua n kh acetylen trong 5 pht c mt
ng nn ti bc sng 279,5 nm. Trong cng mt cch,
ht mt phn ca dung dch chun v lu kt qu. Cui
cng, ht dung dch mu v so snh kt qu vi kt qu
ca dung dch chun, v nhn gi tr ny vi 20 c
c nng tnh bng mg mangan/kg mu ban u
c ly phn tch.


QCVN 4 - 18 : 2011/BYT
17
Phosphor c m t trong Ct 3 ca Bng 1.
Ho cht, thuc th:
Dung dch amoni molybdat 5%: Ho 50 g amoni molybdat
tetrahydrat, (NH
4
)
6
Mo
7
O
24
4H
2
O, trong 900 ml nc m,
lm ngui ti nhit phng, pha long ti 1000 ml bng
nc v lc u.
Dung dch amoni Vanadat 0,25%: Ho 2,5 g amoni
metavanadat, NH
4
VO
3
, trong 600 ml nc si, lm ngui
ti 60 70
0
C v thm vo 20 ml dung dch acid nitric. Lm
ngui ti nhit phng, pha long ti 1000 ml bng
nc v lc u.
Dung dch km acetat 10%: Ho 120 g km acetat
dihydrat, Zn(C
2
H
3
O
2
)
2
,H
2
O, trong 880 ml nc v lc qua
giy lc Whatman s 2V hoc giy lc tng ng trc
khi s dng.
Dung dch acid nitric 29%: Thm 300 ml dung dch acid
nitric (t trng 1,42) vo 600 ml nc v lc u.
Dung dch phosphor chun (100 g P/ml): Ho 438,7 mg
KH
2
PO
4
trong nc trong bnh nh mc 1000 ml, pha ti
1000 ml bng nc v lc u.
ng chun:
Dng pipet ht 5; 10 v 15 ml dung dch phosphor chun
cho vo cc bnh nh mc ring bit dung tch 100 ml.
Thm vo mi bnh v bnh mu trng th t ln lt theo
th t 10 ml dung dch acid nitric, 10 ml dung dch amoni
Vanadat v 10 ml dung dch amoni molybdat, lc mnh
sau mi khi thm. Pha ti th tch 100 ml bng nc, lc
u v yn trong 10 pht. o hp th ca mi dung
dch chun trong cng o 1 cm bc sng 460 nm bng
thit b quang ph thch hp, s dng mu trng t gi
tr hp th trn thit b bng 0. V ng chun trn
th biu din hp th vi nng tng dung dch (mg
P/100 ml).
X l mu s b:
Cho 20 25 g mu tinh bt vo cc dung tch 250 ml;
thm vo 200 ml hn hp methanol/nc (7/3), phn tn
mu v lc bng my trong 15 pht. Thu hi tinh bt bng
cch lc chn khng vo phu thy tinh xp c l xp
trung bnh dung tch 150 ml hoc phu Buchner, v ra
bnh tinh bt m bng 200 ml hn hp methanol/nc.
Li chuyn bnh tinh bt m thnh bt nho trong dung
mi, ra ln hai theo cch tng t. Sy bnh tinh bt lc
trong t sy nhit nh hn 50
0
C, sau nghin mu
qua ry 20 mesh hoc mn hn v trn u. Xc nh hm
lng cht kh bng cch sy mt phn 5 g trong t sy
QCVN 4 - 18 : 2011/BYT
18
chn khng, khng qu 100 mmHg, 120
0
C trong 5 gi.
(Ch : x l c a ra trn ph hp vi cc sn
phm tinh bt khng tan trong nc lnh. i vi tinh bt
c h ha trc v cc loi tinh bt tan trong nc
khc, chun b dung dch bt nho 1 2% trong nc, sau
cho vo ng cellophan v thm tch nc ct lin tc
trong 30 40 gi. Kt ta tinh bt bng cch dung dch
vo 4 phn th tch aceton/1 phn th tch dung dch bt
nho ng thi khuy. Thu hi tinh bt bng cch lc chn
khng vo phu thu tinh xp c l xp trung bnh hoc
phu Buchner, ra bnh lc bng ethanol tuyt i. Sy
bnh lc v xc nh hm lng cht kh theo hng dn
i vi cc tinh bt khng tan trong nc.
Chun b mu:
Cn chnh xc 10 g mu x l s b, tnh theo cht
kh, cho vo a Vycor v thm vo 10 ml dung dch km
acetat, phn tn dung dch u trong mu. C n kh
trn tm gia nhit sau tng nhit v carbon ho mu
trn tm gia nhit hoc trn ngn la gas. t chy trong
l nung 550
0
C cho n khi tro khng cn carbon
(khong 1 2 gi), lm ngui. Lm m tro bng 15 ml
nc v ra chm xung thnh a bng 5 ml dung dch
acid nitric. Gia nhit n si, lm ngui v chuyn ton
lng hn hp vo bnh nh mc dung tch 200 ml, ra
a bng ba phn 20 ml nc v cho nc ra vo bnh.
Pha ti th tch 200 ml bng nc v lc u. Chuyn mt
lng chnh xc (V ml) ca dung dch ny, cha khng
c qu 1,5 mg P, vo trong bnh nh mc dung tch
100 ml v thm vo 10 ml dung dch acid nitric, 10 ml dung
dch amoni Vanadat v 10 ml dung dch amoni molybdat,
lc u sau mi ln thm. Pha ti th tch 100 ml bng
nc, lc u v yn trong 10 pht.
Cch tin hnh:
o hp th ca dung dch mc Chun b mu trong
cng o 1 cm bc sng 460 nm bng thit b quang
ph ph hp, s dng mu trng ci t thit b 0. T
ng chun, xc nh s mg phosphor trong lng mu
ly, ghi li gi tr ny l a. Tnh hm lng mg P/kg mu
gc theo cng thc sau:

Trong :
W: Khi lng mu th (g)
QCVN 4 - 18 : 2011/BYT
19
Cc nhm acetyl c m t trong Ct 3 ca Bng 1.
Cn chnh xc 5 g mu v cho vo bnh nn dung tch 250
ml. To hn dch trong 50 ml nc, thm vo vi git
phenolphthalein TS v chun bng dung dch NaOH
0,1N n khi xut hin mu hng nht. Thm 25 ml dung
dch NaOH 0,45N, y np bnh v lc mnh trong 30
pht, thch hp nht l lc bng my. (Ch : Nhit
khng c qu 30
0
C, nu khng mt vi loi tinh bt c
th b h ha). Tho np y, ra np v thnh bnh bng
mt vi ml nc v chun kim d bng dung dch HCl
0,2N cho n khi mt mu hng. Ghi li th tch dung dch
HCl 0,2N dng chun (S ml). Thc hin chun
mu trng trn 25 ml dung dch NaOH 0,45N v ghi li th
tch ca dung dch HCl 0,2N (B ml)
(B S) x N x 0,043 x 100
% cc nhm acetyl = -------------------------------------------
W
Trong :
N: Nng ng lng ca dung dch HCl
W: Khi lng mu (g)
QCVN 4 - 18 : 2011/BYT
20
Vinyl acetat Xc nh bng phng php sc k kh khng gian hi.
S dng thit b sc k kh c trang b ct thu tinh nhi
Porapak Q 80 100 mesh (hoc tng ng) c chiu
di 2 m, ng knh trong 2 mm; detector ion ho ngn
la; thc hin vi cc iu kin sau:
- Tc dng kh mang (nitrogen): 20 ml/pht
- Nhit cng bm mu: 200
0
C
- Nhit ct: 50
0
C
- Nhit detector: 200
0
C
Chun b chun: Cn chnh xc 150 mg vinyl acetat (tinh
khit) cho vo bnh nh mc dung tch 100 ml. Ho tan v
nh mc n th tch 100 ml bng nc ct. Cho 1 ml
dung dch ny vo bnh nh mc dung tch 10 ml v nh
mc ti 10 ml bng nc ct. Thm 1 ml dung dch long
ny vo 30 g tinh bt cha bin tnh ca cng ngun gc
thc vt nh l cht th trong bnh dung tch 100 ml c
np giong. ng kn bnh ngay lp tc bng np giong.
Cch lm ny thu c tinh bt chun vi hm lng vinyl
acetat 5 mg/kg.
Cch tin hnh:
Cn 30 g cht th cho vo trong bnh nh mc dung tch
100 ml c np giong. ng kn bnh. bnh c cha
cht th v bnh c cha tinh bt chun chu nc c
nhit khng i 70
0
C trong 30 pht. Ly 2 ml t th tch
kh trong bnh cha chun, s dng syringe (xylanh) kn,
bm trc tip vo cng bm ca thit b sc k kh v ghi
chiu cao pick ca sc ph. Tng t bm 2 ml th tch
kh t bnh cha cht th vo thit b sc k. Tnh hm
lng vinyl acetat trong cht th t vic so snh chiu cao
cc pick ca hai sc k .
QCVN 4 - 18 : 2011/BYT
21
Cc nhm adipat c m t trong Ct 3 ca Bng 1.
Ho cht v dung dch:
N,N-Bis-trimethylsilyltrifluoroacetamid (BSTFA): ca
Macherey-Nagel, D 5160 Dueren, c hoc tng ng.
Dung dch acid glutaric: Ho tan 1 g acid glutaric (ca
Merck hoc tng ng) trong nc v pha ti 1.000 ml.
Dung dch acid adipic: Ho tan 1 g acid adipic (UCB,
Brussels, B hoc tng ng) trong 900 ml nc m,
lm ngui n nhit phng, pha ti 1.000 ml v lc
u.
Dng c, thit b:
Thit b sc k kh Hewlett-Packard Model 7620A hoc
tng ng c trang b detector ion ho ngn la v
Thit b phn tch Model 3370A.
Cc thng s ct: lm bng thp khng r c chiu di 2 m,
ng knh trong 1,83 mm, c nhi bng OV-17 5%
trn Chromosorb GAW-DMCS 80 - 100 mesh (Alltech
Europe, Inc,. B 9731 Eke, B); luyn ct 350
0
C trong 24
gi vi tc kh mang nitrogen 40 ml/pht. Cc tc
dng kh hot ng (ml/pht): kh mang nitrogen l 30,
hydrogen l 40, khng kh l 400. Nhit : bung bm
mu 280
0
C, detector 250
0
C, ct 140
0
C. Cc thi gian lu
(pht): acid glutaric l 2,83; acid adipic l 4,5.
Hiu chun:
Cn v cho vo 4 bnh Erlenmeyer dung tch 250 ml (1 g
tinh bt ng dng sp/bnh). Thm vo mi bnh 50 ml
nc v 1 ml dung dch nc cha 1 mg acid glutaric/ml.
Thm vo bnh mt 0,25 ml dung dch nc cha 1 mg
acid adipic/ml, thm vo 3 bnh cn li ln lt 0,5; 0,75
v 1 ml. Mi bnh sau cha 1 mg acid glutaric v ln
lt l 0,25; 0,5; 0,75 v 1 mg acid adipic. Lc mnh cc
bnh bng tay phn tn hon ton tinh bt v thm 50
ml dung dch NaOH 4N. Tip tc lc mnh trong 5 pht,
mi bnh trong chu nc nhit mi trng v thm
cn thn 20 ml dung dch HCl 12N cho mi bnh. Khi mi
bnh ngui, chuyn ton lng hn hp trong bnh vo
phu chit dung tch 250 ml. Chit vi 100 ml ethyl acetat
tinh khit. Rt lp nc di vo mt cc vi ; tp trung
lp dung mi hu c pha trn vo mt bnh Erlenmeyer
dung tch 500 ml cha 20 g Na
2
SO
4
khan. Chuyn phn
QCVN 4 - 18 : 2011/BYT
22
tan trong nc quay tr li phu chit v lp li chit bng
ethyl acetat hai ln na. Lc cc bnh nh k trong 10
pht v sau lc qua giy lc Whatman s 1 vo trong
cc bnh y trn dung tch 1 lt. Ra cc bnh v cc cn
khng ho tan c lc 2 ln bng 50 ml ethyl acetat. C
ton b phn chit hu c v cc nc ra ca mi bnh
nhit khng qu 40
0
C, p sut chn khng (50
mgHg) cho n khi kh hon ton.
C ethyl acetat nn c thc hin cng nhanh cng tt
bi v d xy ra cc phn ng thu phn trong qu trnh.
Cc sn phm thu phn lm gim phn gii ca acid
adipic trong phn tch sc k.
Thm ln lt 2 ml pyridin v 1 ml N,N-Bis-
trimethylsilyltrifluoroacetamid vo cc thnh phn kh. y
np tng bnh y trn v ra b mt bn trong tht k
bng cch lc xoy. yn cc bnh trong 1 gi sau
chuyn khong 2 ml t mi bnh vo cc l thu tinh nh
v y kn ngay lp tc. Bm 4 l vo thit b sc k kh.
Tnh kt qu:
Xc nh cc thi gian lu i vi mi acid v xc nh
chiu cao pic i vi acid glutaric v i vi mi nng
acid adipic. V th biu din quan h tuyn tnh gia t
l chiu cao pic ca acid adipic/chiu cao pic ca acid
glutaric vi hm lng acid adipic. ng hiu chun ny
c th c s dng nhng n gin hn s dng mt h
s p ng (RF):

Trong :
H
s
v H
l
: Cc chiu cao ln lt ca ca acid adipic chun
v acid glutaric;
W
s
: Khi lng acid adipic chun
RF nn c kim tra mi tun mt ln.
Adipat tng s:
Cn chnh xc 1 g mu cho vo bnh Erlenmeyer dung tch
250 ml, thm vo 50 ml nc v 1 ml dung dch tan trong
nc c 1 mg acid glutaric/ml. Tin hnh nh trong phn
Hiu chun, bt u Lc cc bnh bng tay....
Acid adipic t do:
Cn chnh xc 5 g mu cho bnh Erlenmeyer dung tch
250 ml, thm vo 100 ml nc v 1 ml dung dch acid
glutaric. Lc mnh trong 1 gi, lc qua dng c lc
Milipore 0,45 m, thm 1 ml dung dch HCl m c vo
phn lc c v chuyn ton lng vo phu chit dung
QCVN 4 - 18 : 2011/BYT
23
tch 250 ml. Tin hnh nh trong phn Hiu chun, bt
u Chit vi 100 ml....
Tnh kt qu:
i vi c hai php nh lng (Hm lng adipat tng
v Hm lng acid adipic t do) ghi chiu cao cc pic
i vi acid adipic v acid glutaric (ni chun). Tnh hm
lng ln lt adipat tng s v acid adipic t do c trong
mu theo cng thc sau:

Trong :
A: Hm lng adipat tng s hoc acid adipic t do (%)
H
X
: Chiu cao pic ca acid adipic trong dung dch mu
thc
H
IX
: Chiu cao pic ca acid glutaric trong dung dch mu
thc
RF: H s p ng i vi acid adipic
S: Khi lng mu trong dung dch mu thc (g)
Cc nhm adipat (%) = Hm lng adipat tng s (%)
hm lng acid adipic t do (%)
QCVN 4 - 18 : 2011/BYT
24
Cc nhm hydroxypropyl c m t trong Ct 3 ca Bng 1.
Thuc th Ninhydrin:
Dung dch 3% tinh th 1,2,3,-triketohydrinden trong dung
dch natri bisulfit 5% trong nc.
Cch tin hnh:
Cn chnh xc 50 100 mg mu cho vo trong bnh nh
mc dung tch 100 ml v thm 25 ml dung dch H
2
SO
4
1N.
Chun b mt mu tinh bt cha bin tnh c cng ngun
gc (tc l ng hoc khoai ty) trong cng cch thc hin.
t cc bnh trong cch thy si v gia nhit cho n khi
cc mu to thnh dung dch. Lm ngui v pha ti th
tch 100 ml bng nc. Nu cn thit pha long mu hn
m bo khng c qu 4 mg nhm hydroxypropyl/100
ml, sau pha mu trng tinh bt tng ng. Dng pipet
ly 1 ml cc dung dch cho vo cc ng th nh mc 25
ml c cc np thu tinh c ngm trong nc lnh, thm
tng git 8 ml dung dch H
2
SO
4
m c vo mi ng. Lc
u v t cc ng trong cch thy si chnh xc 3 pht.
Chuyn ngay lp tc cc ng vo chu cho n khi
dung dch lnh. Thm 0,6 ml ninhydrin, cn thn cho
thuc th chy xung theo thnh ca cc ng th. Lc
u ngay lp tc v t cc ng trong chu nc 25
0
C
trong 100 pht. iu chnh th tch trong mi ng ti 25 ml
bng acid H
2
SO
4
v lc ngc cc ng vi ln. (Khng
c lc). Ngay lp tc chuyn cc phn ca cc dung
dch vo cc cng o 1 cm v sau chnh xc 5 pht o
hp th (A) bc sng 590 nm, s dng mu trng tinh
bt nh l mu i chng. Chun b ng chun bng
cc phn 1 ml ca cc dung dch chun tan trong nc c
10, 20, 30, 40 v 50 g propylen glycol/ml.
Tnh kt qu:
C x 0,7763 x 10 F
Cc nhm hydroxypropyl (%) =-----------------------------
W
Trong :
C: Hm lng propylen glycol trong dung dch mu tnh
c da vo ng chun ( g/ml)
F: H s pha long (nu cn mt pha long hn)
W: Khi lng mu (mg)
Propylen clorhydrin c m t trong Ct 3 ca Bng 1.
Thit b sc k kh:
S dng thit b Hewlett-Packard Model 5750 hoc tng
ng. Mt thit b ct kp c trang b detector ion ho
ngn la. Mt thit b tch phn l mt phn ca h thng
QCVN 4 - 18 : 2011/BYT
25
ghi.
Ct sc k kh: S dng ct thp khng r, di 3 m, ng
knh ngoi 3,2 mm, c nhi 10% Carbowax 20M trn
80/100 mesh Gas Chrom 2, hoc tng ng. Sau khi
nhi, trc khi s dng, luyn ct qua m trong iu kin
nhit 200
0
C, s dng dng kh heli vi tc 25
ml/pht.
Dng c c c: S dng dng c c c Kuderna-Danish
c mt bnh dung tch 500 ml, c sn ca Cng ty Kontes
Glass,.. Vineland, N.J., M, (Catalog s K-57000), hoc
tng ng.
Cc bnh p lc: S dng cc bnh p lc dung tch 200
ml, c giong Neoprene, np y thu tinh v gn vi mt
ci kp kim loi, c sn ca Cng ty Fisher Scientific,
Pittsburgh, PA, M. (Vitro 400, catalog s 3 100). hoc
tng ng.
Ho cht, thuc th:
Diethyl ether: S dng diethyl ether khan, tinh khit dnh
cho phn tch.
Florisil: S dng vt liu 60/100 mesh, c sn ca Cng ty
Floridin, 3 Penn Center, PA 15235, M, hoc sn phm
tng ng.
Propylen chlorohydrin: S dng Eastman s P1325 1-
Chloro-2-propanol thch hp, cha 25% 2-chloro-1-
propanol, c sn ca Cng ty Eastman Kodak, Rochester,
N.Y.14650, M hoc tng ng.
Chun b dung dch chun: Ly 25 l hn hp cc ng
phn propylen chlorohydrin cha 75% 1-chloro-2-propanol
v 25% 2-chloro-1-propanol cho vo syringe (xylanh) dung
tch 50 l. Cn chnh xc syringe v bm mt phn vo
bnh nh mc dung tch 500 ml, cha mt phn nc.
Cn li syringe v ghi trng lng cc chlorohydrin ly.
Pha ti th tch 500 ml bng nc v lc u. Dung dch
ny cha khong 27,5 mg hn hp cc chlorohydrin, hoc
khong 55 g/ml. Chun b dung dch ny mi trong ngy
s dng.
Chun b mu th:
Cho 50 g mu i din c trn vo Bnh p lc v
thm vo 125 ml dung dch H
2
SO
4
2N. Kp v tr pha trn
bnh v lc xoy hn hp cho n khi mu c phn tn
hon ton. t bnh trong cch thy si, gia nhit trong 10
pht sau lc xoy bnh trn cc thnh phn, v gia
nhit trong cch thy thm 15 pht na. Lm ngui trong
khng kh ti nhit phng sau trung ho mu thu
QCVN 4 - 18 : 2011/BYT
26
phn ti pH = 7 bng dung dch NaOH 25% v lc qua
giy lc Whatman s 1, hoc tng ng, vo phu
Buchner, s dng lc ht. Ra bnh v giy lc bng 25
ml nc v tp hp cc nc ra vi phn lc c.
Thm vo 30 g Na
2
SO
4
khan v khuy bng my khuy t
trong 5 10 pht, hoc cho n khi Na
2
SO
4
c ho tan
hon ton. Chuyn dung dch ny vo mt phu tch dung
tch 500 ml c trang b vi kho teflon, ra bnh bng
25 ml nc v tp hp cc nc ra vi dung dch mu.
Chit vi 5 phn x 50 ml diethyl ether, t nht 5 pht
trong mi qu trnh chit tch pha hon ton. Chuyn
cc phn dch chit ether vo dng c c c, t bnh
hng chia ca dng c c c trong cch thy duy tr
50 55
0
C v c c dch chit ti th tch 4 ml.
(Ch : Dch chit ether ca mu c th cha tp cht l
gy tr ngi n phn tch v/hoc bin gii cc sc .
Cc tp cht ny l cc sn phm c sinh ra trong qua
trnh thu phn. Cc kh khn phn tch to ra bi s xut
hin ca cc tp cht c th trnh c thng qua vic
s dng bin php x l lm sch sau:
C c dch chit ether ti 8 ml, thay v 4 ml nh
cp trn. Thm vo 10 g Florisil, trc c gia nhit
n 130
0
C trong 16 gi ngay trc khi dng, vo ct sc
k c kch thc thch hp, sau v nh v thm vo 1 g
Na
2
SO
4
khan vo nh trn ca ct. Lm m ct bng 25
ml diethyl ether v chuyn ton lng dch chit c c
vo ct vi s tr gip ca cc phn nh ether. Ra gii
bng 3 phn x 25 ml ether, ly tt c phn ra gii chuyn
vo dng c c c v c c n 4 ml).
Lm ngui dch chit ti nhit phng, chuyn ton
lng vo bnh nh mc dung tch 5 ml vi s h tr ca
cc phn nh diethyl ether, pha ti th tch 5 ml bng
ether v lc u.
Chun b mu i chng:
Chuyn cc phn 50 g tinh bt ng dng sp cha bin
tnh (cha c chuyn ho) vo 5 bnh p lc ring bit
v thm vo mi bnh 125 ml dung dch H
2
SO
4
2N. Thm
0; 0,5; 1; 2 v 5 ml dung dch chun ln lt vo cc bnh,
c c cc nng propylen chlorohydrin so vi tinh
bt ln lt l 0; 0,5; 1; 2 v 5 mg/kg. Tnh nng chnh
xc trong mi bnh t trng lng cc propylen
chlorohydrin s dng trong cch lm Chun b dung
dch chun. Kp vo v tr u bnh, lc xoy cho n khi
cc cht trong mi bnh c ho tan hon ton, tin hnh
thu phn, trung ho, lc, chit, c phn dch chit v cui
QCVN 4 - 18 : 2011/BYT
27
cng pha nh hng dn trong phn Chun b mu th.
Cch tin hnh:
Cc iu kin vn hnh c th khc nhau ph thuc vo
thit b c th s dng, nhng sc ph hp thu c
bng thit b Hewlett-Packard Model 5750 s dng nhit
ct 110
0
C ng nhit; nhit cng bm 210
0
C; nhit
detector 240
0
C; tc dng kh hydrogen 30 ml/pht;
tc dng kh heli 25 ml/pht, hoc tc khng kh 350
ml/pht nh kh mang. C b ghi n 1 mV; tc sp
xp, lm long v giy ghi c la chn ti u ho
cc c tnh tn hiu. Bm cc phn 2 l ca mi dch
chit c c c chun b theo hng dn trong phn
Chun b mu i chng, thi gian gia cc ln
bm i vi cc pic tn hiu tng ng vi hai ng phn
chlorohydrin ghi c (v tch phn c) v ct c
lm sch. Ghi v tnh tng cc din tch tn hiu (thit b
phn tch tn hiu ra) t hai ng phn chlorohydrin i vi
mi mu i chng. S dng cc iu kin hot ng
thng nht, bm 2 l phn chit c c chun b theo
hng dn trong phn Chun b mu th, ghi v tnh tng
cc din tch tn hiu (thit b phn tch tn hiu ra) t mu
th.
Tnh kt qu:
Chun b th ng chun trn giy bng cch v cc
din tch tn hiu tng ca mi mu i chng vi cc
nng propylen chlorohydrin (mg/kg), xut pht t trng
lng thc ca ng phn chlorohydrin s dng. S dng
cc din tch tn hiu tng tng ng vi 1-chloro-2-
propanol v 2-chloro-1-propanol t mu th, xc nh
nng ca hn hp cc propylen chlorohydrin (mg/kg)
trong mu th lin quan ti th ng chun xut pht
t cc mu i chng. Sau khi c c kinh nghim v
cch tin hnh v biu th c th ng chun t cc
mu i chng tuyn tnh v lp li, s mu i chng c
th c gim n mt mu c cha khong 5 mg/kg hn
hp cc ng phn propylen chlorohydrin. Hm lng
propylen chlorohydrin trong mu khi c th c tnh
theo cng thc sau:

Trong :
C: Nng (mg/kg) ca cc propylen chlorohydrin (tng
ca cc ng phn) trong mu i chng
a: Tng din tch tn hiu c to ra bi cc ng phn
propylen chlorohydrin trong mu th
QCVN 4 - 18 : 2011/BYT
28
A: Tng din tch tn hiu c to ra bi cc ng phn
propylen chlorohydrin trong i chng
QCVN 4 - 18 : 2011/BYT
29
ester ha ca natri
octenyl succinat tinh bt
Nguyn tc:
ester ha c xc nh bi lng kim tiu th sau
khi acid ho v ra k monoester ca acid octenylsuccinic
vi tinh bt.
Cch tin hnh:
Cn v cho 5 g mu vo cc dung tch 150 ml. Lm m
bng mt vi ml isopropyl alcol tinh khit. Dng pipet thm
vo 25 ml dung dch HCl 2,5N trong isopropanol, dng
acid ra mu bm trn thnh cc. Khuy trong 30 pht
bng my khuy t. Thm vo 100 ml isopropanol 90% t
ng ong chia . Khuy trong 10 pht. Lc mu qua phu
Buchner v ra bnh lc bng isopropanol 90% cho n
khi dch lc thu c khng cn ion clorid. S dng
AgNO
3
0,1N kim tra cc ion clorid. Chuyn bnh lc
vo cc dung tch 600 ml v ra nh phu Buchner ra
tinh bt trong cc. Thm nc ct vo cho n th tch
300 ml. t trong cch thy si c khuy trong 10 pht.
Chun trong khi cn nng bng dung dch NaOH 0,1N
cho n im kt thc c pht hin bng
phenolphthalein.
Kt qu:
0,162 x A
ester ha (DS) = -------------------------
1 0,210 x A
Trong :
A: s mili ng lng ca NaOH s dng/g octenyl
succinat tinh bt
D lng acid octenyl
sucinic trong natri octenyl
sucinat tinh bt
Chit xut v chun b dung dch mu:
Chit xut khong 500 mg tinh bt vi 15 ml methanol qua
m vi lc thng xuyn (cn chnh xc lng tinh bt).
Lc hn hp chit. Ra tinh bt trn dng c lc bng 7 ml
methanol. Lp li 3 ln. Tp hp cc phn dch lc
(khong 80% d lng c chit xut bi cch lm ny).
Thm vo cc phn dch chit thu c 1 ml KOH 0,16N
trong methanol. Lm kh cc phn dch chit thu c
bng thit b c nhanh 30
0
C. Ho tan cn thu c trong
2 ml methanol. Ly 0,5 ml dung dch cn cho vo l phn
ng. Thm vo l phn ng 0,5 ml thuc th to dn xut
(2,8 g 2-p-dibromoacetophenon v 0,28 g 18-Crown-6
trong 50 ml CH
3
CN). Thm 2 ml CH
3
CN vo l phn ng.
y np kn l phn ng v gia nhit 80
0
C trong 30
pht. Lm ngui dung dch phn ng n nhit phng
(s dng trong 24 gi).
Phn tch sc k lng:
- Ct: Micro-Bondapark C
18
(Waters) hoc tng ng
QCVN 4 - 18 : 2011/BYT
30
- Pha ng: ra gii Gradient methanol 70% trong nc
n methanol 80% trong nc trong 5 pht. ng 6
(thit b lp trnh dung mi Waters 660).
Tc dng: 1,5 ml/pht
Detector: UV ti bc sng 254 nm, tt dn 0,16 AUFS
Th tch bm: 5 l
Chun b ng chun:
Chun b dung dch natri octenyl succinat 0,5 M (Dung
dch A). Ly 0,25 ml Dung dch A bng syringe cho vo
bnh nh mc dung tch 25 ml. Pha ti 25 ml bng
methanol (Dung dch B). Chun b ba chun hiu chun
bng cch ly 0,5; 1 v 2 ml Dung dch B cho vo 3 bnh
y trn dung tch 50 ml. Thm vo mi bnh 1 ml dung
dch KOH 0,16N trong methanol. Lm kh mi dung dch
bng thit b c nhanh 30
0
C. Ho tan cn thu c trong
2 ml methanol (Dung dch C
1
, C
2
v C
3
). Cho 0,5 ml dung
dch cn vo l phn ng. Thm 0,5 ml thuc th to dn
xut (2,8 g 2-p-dibromoacetophenon v 0,28 g 18-Crown-6
trong 50 ml CH
3
CN) vo l phn ng. Thm vo 2 ml
CH
3
CN. y np kn v gia nhit ti 80
0
C trong 30 pht.
Lm ngui dung dch phn ng n nhit phng (cht
dn xut nn c chun b khi cn v s dng ngay).
Bm 5 l vo thit b sc k lng. Hm lng cht tn d
trong mi ln bm 5 l nh sau:
i vi Dung dch C
1
0,2375 g
i vi Dung dch C
2
0,4750 g
i vi Dung dch C
3
0,9500 g
V th biu din mi tng quan gia chiu cao pic thu
c t trn sc k vi g cht tn d/5 ml dung dch.
Tnh kt qu:
Chun b ng chun da vo cch tin hnh. S dng
chiu cao pic ca mu cha bit t sc k , xc nh
hm lng cht tn d (tnh theo acid octenyl succinic)
trong th tch bm t ng chun.
300 x gi tr t th
% Cht tn d trong tinh bt = -------------------------------------
--
Khi lng tinh bt (mg)
Ghi ch: Cng thc ny c hiu chnh v thu hi
100% bng cch chia cho 0,80; do vy 240/0,80 = 300.