Chat Nhu Hoa

QCVN 4-22:2011/BYT
QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT NH HA
National technical regulation on Food Additive Emulsifier
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 cht nh ha 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
cht nh ha 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. Cht nh ha: l ph gia thc phm c b sung vo thc phm nhm
mc ch to ra hoc duy tr dng nh tng ng nht ca hai hay nhiu thnh
phn ca thc phm.
3.2. 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.
3.3. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.4. TS (test solution): Dung dch thuc th.
3.5. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.6. MTDI
3.6. INS (International numbering system): H thng m s quc t v ph gia
thc phm.
QCVN 4-22: 2011/BYT

II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht nh ha c quy
nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1.
Ph lc 1:
1.2.
Ph lc 2:
1.3.
Ph lc 3 :
1.4.
Ph lc 4:
1.5.
Ph lc 5:
1.6.
Ph lc 6:
1.7.
Ph lc 7:
1.8.
Ph lc 8:
1.9.
Ph lc 9:
1.10.
Ph lc 10:
1.11.
Ph lc 11:
1.12.
Ph lc 12:
1.13.
Ph lc 13:
1.14.
Ph lc 14:
1.15.
Ph lc 15:
1.16.
Ph lc 16:
1.17.
Ph lc 17:
1.18.
Ph lc 18:
1.19.
Ph lc 19:
1.20.
Ph lc 20:
Yu cu k thut v phng php th i vi monov di-glycerid ca acid bo

Yu cu k thut v phng php th i vi ester
ca glycerol vi acid lactic v acid bo
ca glycerol vi acid citric v acid bo
ca glycerol vi acid diacetyl tartric v acid bo
Yu cu k thut v phng php th i vi
sucroglycerid
ca polyglycerol vi cc acid bo
Yu cu k thut v phng php th i vi stearyl
citrat
Yu cu k thut v phng php th i vi trikali
ortho-phosphat
Yu cu k thut v phng php th i vi cc
mui amoni ca acid phosphatidic
Yu cu k thut v phng php th i vi sucrose
acetat isobutyrat
glycerol ca nha cy
Yu cu k thut v phng php th i vi dinatri
diphosphat
Yu cu k thut v phng php th i vi calci
polyphosphat
Yu cu k thut v phng php th i vi cc
mui ca acid myristic, palmitic v stearic (Ca, Na, K,
NH4)
ca sucrose vi cc acid bo
Yu cu k thut v phng php th i vi dioctyl
natri sulphosucinat
Yu cu k thut v phng php th i vi stearyl
tartrat
Yu cu k thut v phng php th i vi sorbitan
monostearat
tristearat
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QCVN 4-22: 2011/BYT

1.21.
Ph lc 21:
1.22.
Ph lc 22:
monolaurat
monooleat
monopalmitat
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 cc 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 cht nh ha 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.
2. Kim tra i vi cht nh ha
Vic kim tra cht lng, v sinh an ton i vi cc cht nh ha 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 cht nh ha 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.
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QCVN 4-22: 2011/BYT

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 4-22: 2011/BYT

Ph lc 1
YU CU K THUT V PHNG PHP TH
I VI MONO V DIGLYCERID CA CC ACID BO
1. Tn khc, ch s
Glyceryl monostearate, glyceryl monopalmitate, glyceryl

monooleate; monostearin, monopalmitin, monoolein; GMS
(i vi glyceryl monostearate);
INS 471
2. nh ngha
Hn hp cc ester mono- v diglyceryl mch di vi cc acid

bo bo ha v khng bo ha c trong cht bo thc phm;
c cha hm lng alpha-monoglycerid khng thp hn 30%
v cng c th c cha cc monoglycerid ng phn; cng
nh di- v triglycerid, glycerol t do, cc acid bo t do, sn
phm x phng ha v nc; thng c sn xut bng
cch thy phn tch glyceryl ca cc cht bo v du thc
phm, nhng cng c th c sn xut bng cch este ha
cc acid bo vi glycerol c hoc khng qua chng ct phn
t.
Cng thc cu to
Trong OCR l ca acid bo

Khi lng phn t
Glyceryl monostearat: 358,6

Glyceryl distearat: 625,0
3. Cm quan
Cht bo rn dng sp c mu trng hoc kem hoc dng

lng snh
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, tan trong ethanol, cloroform v

benzen.
Hp th hng ngoi
Phi c ph hng ngoi c trng ca ester mt phn ca

acid bo vi polyol.
Phi c phn ng c trng ca acid bo.
Acid bo
Glycerol
Phi c phn ng c trng ca glycerol.
5.2. tinh khit

Nc
Khng c qu 2,0 % (phng php Karl Fischer)
QCVN 4-22: 2011/BYT

Ch s acid
Khng c qu 6.
Glycerol t do
Khng c qu 7%
X phng
Khng c qu 6%, tnh theo natri oleat.
Ch
Khng c qu 2,0 mg/kg.
6. Phng php th
tinh khit
X phng
Thm 10 g mu th vo hn hp gm 60 ml aceton v 0,15

ml dung dch xanh bromophenol (0,5%) c trung ha
trc bng acid hydrocloric 0,1N hoc natri hydroxyd 0,1N.
Lm m t t trn cch thy cho n khi dung dch tan hon
ton, chun bng acid hydrocloric 0,1N cho n khi mu
xanh bin mt. yn dung dch trong 20 pht, lm m cho
n khi cn c ha tan v mu xanh ti xut hin, tip tc
chun n mt mu xanh.
Mi ml acid hydrocloric 0,1N tng ng vi 0,0304 g
C18H33O2Na.
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.
QCVN 4-22: 2011/BYT

Ph lc 2
I VI ESTER CA GLYCEROL VI ACID LACTIC V ACID BO
1. Tn khc, ch s
Lactic acid esters of mono- and diglycerides; lactoglycerides

INS 472b
2. nh ngha
L hn hp cc ester ca glycerol vi acid lactic v acid bo

trong cht bo thc phm.
Sn phm thng mi c th ch r hm lng monglycerid,
acid lactic, ch s acid, ch s x phng ha, hm lng acid
bo t do, im ng c ca cc acid bo t do, ch s iod,
hm lng glycerol t do v hm lng nc.
Cng thc cu to
Trong R1, R2 v R3 l ca acid bo, acid lactic hoc

hydrogen (theo thnh phn)
3. Cm quan
Cht rn dng sp
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc lnh nhng c th phn tn trong nc

nng.
Acid bo
Acid lactic
Glycerol
Phi c phn ng c trng ca acid lactic.

5.2. tinh khit

Cc acid
Ch c acid bo v acid lactic.
Ch
6. Phng php th
tinh khit
Ch

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QCVN 4-22: 2011/BYT

Ph lc 3
I VI ESTER CA GLYCEROL VI ACID CITRIC V ACID BO
1. Tn khc, ch s
Citric acid esters of mono- and di-glycerides, citroglycerides,

CITREM;
INS 472c
2. nh ngha
Thu c nh qu trnh ester ho glycerol vi acid citric v

acid bo thc phm hoc nh phn ng ca hn hp mono
v diglycerid ca acid bo vi acid citric; ch phm bao gm
cc ester hn hp ca acid citric v cc acid bo vi
glycerol; c th cha lng nh cc acid bo t do, glycerol
t do, acid citric t do v mono v diglycerid; c th c
trung ho hon ton hoc mt phn bng NaOH hoc KOH
(nh c cng b trn nhn mc).
Cng thc cu to
Trong : t nht mt trong R 1, R2 hoc R3 l ca acid citric,

mt l ca acid bo v R cn li c th l ca acid citric,
acid bo hoc hydrogen.
3. Cm quan
Dng du ti sp, mu trng n trng ng
4. Chc nng
Cht n nh, cht nh ho, cht chng oxy ho
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc lnh, c th phn tn trong nc

nng; tan trong du v m; khng tan trong ethanol lnh
Acid bo
Phi c phn ng c trng ca acid bo .
Acid citric
Glycerol
Phi c phn ng c trng ca acid citric.

5.2. tinh khit

Tro sulfat
Sn phm khng c trung ho : Khng c qu 0,5%

Sn phm c trung ho hon ton hoc mt phn: Khng
c qu 10%
(S dng 2 g mu th, phng php I)
Glycerol t do
Khng c qu 4%
Glycerol tng s
8 33% (m t trong phn Phng php th)
Acid citric tng s
Acid bo tng s

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QCVN 4-22: 2011/BYT
Ch
6. Phng php th
tinh khit
Glycerol tng s
Cn chnh xc 2 g mu v cho vo bnh x phng ho, thm

vo 50 ml dung dch KOH 0,5 M trong ethanol, v un si
vi sinh hn ngc trong 30 pht. Thm chnh xc 99 ml (t
buret) chloroform v 25 ml acid acetic bng vo bnh nh
mc dung tch 1 lt. Chuyn ton lng dch trong bnh x
phng ho vo bnh nh mc dung tch 1 lt, cho 3 ln 25
ml nc. Thm vo 500 ml nc v lc mnh trong 1 pht.
Pha n th tch 1 lt bng nc, lc u v yn cho tch
thnh cc lp.
Dng pipet ly 50 ml dung dch acid acetic periodic TS vo
trong cc cc dung tch 400 ml. Chun b 2 mu trng bng
cch thm 50 ml nc vo mi cc. Dng pipet ly 50 ml
dung dch mu trong nc cho vo mt trong cc cc cha
50 ml acid acetic periodic TS, lc nh cho u, y bng
tm knh nhn qua c v yn trong 30 pht. Nhng
khng c qu 1,5 gi. Thm 20 ml dung dch KI 15%, lc
nh cho u v yn t nht 1 pht nhng khng c
qu 5 pht. Khng c di nh sng trc tip hoc
nh sng trng. B sung 100 ml nc v chun bng
dung dch natri thiosulfat 0,1 N. S dng dng my khuy
lm u dung dch. Tip tc chun cho n khi mt
mu iod nu trong dung dch nc. Thm 2 ml tinh bt TS
v tip tc chun cho n khi mt mu iod trong lp
chloroform c tch ra trong qu trnh chun v mt
mu xanh ca tinh bt iodo trong dung dch nc.
Kt qu: Glycerol tng s (%):
Trong :
B: Lng dung dch natri thiosulfat dng chun mu
trng cha 50 ml nc
S: Lng dung dch natri thiosulfat dng chun mu
th
N: Nng dung dch natri thiosulfat 0,1 N
W: Khi lng mu th c ly bng pipet em chun
v c tnh theo cng thc:
Trong : a: Khi lng mu (g) em x phng ha
Acid citric tng s
Nguyn tc:
Mu c x phng ho bng dung dch KOH trong alcol v
cc acid bo c tch ra bng trch ly. Acid citric c
chuyn thnh cc dn sut trimethylsilyl (TMS) v c
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QCVN 4-22: 2011/BYT

phn tch bng sc k kh lng.
X phng ho:
Cn chnh xc 1 g mu cho vo bnh y trn, thm 25 ml
dung dch KOH 0,5M trong ethanol v un si vi sinh hn
ngc trong 30 pht. Acid ho hn hp bng HCl v cho
bc hi bng my c quay hoc bng phng php thch
hp khc.
Trch ly:
Chuyn ton lng mu trong bnh vo mt bnh gn, s
dng khng qu 50 ml nc v trch ly bng 3 ln 50 ml
heptan, loi b phn dch chit heptan tch ra. Chuyn lp
dung dch nc vo bnh nh mc dung tch 100 ml, trung
ho, pha ti th tch 100 ml bng nc v lc u.
Dn xut ho:
Dng pipet ly 1 ml dung dch pha c trn, 1 ml dung
dch acid tartric (1 mg/ml trong nc) cho vo bnh y trn
c th y np dung tch 10 ml v c n kh. Thm 1 ml
pyridin, 0,2 ml dung dch trimethyl-chlorosilan (TMCS), 0,4
ml hexamethyl-disilazan (HMDS), 0,1 ml n-methyl-ntrimethylsilyl-trifluoroacetamid (MSTFA). y np cht v lc
cn thn c dung dch tan hon ton. Gia nhit bnh
trong t sy 600C trong 1 gi.
Sc k kh:
Bt k sc k kh thch hp c th c dng vi detector
ion ho ngn la v ct (thu tinh, chiu di 1,8 m v ng
knh trong 2 mm), c nhi bng DC-200 10% trn
chromosorb Q (80/100 mesh). Cc iu kin cho sc k kh:
nhit l ct 1650C, nhit bung tim 240 0C, nhit
detector 2400C; tc dng kh mang nitrogen 24 ml/pht.
Cch tin hnh:
Bm 5 l mu cc dn xut TMS. Thi gian lu i vi acid
tartric khong 12 pht v thi gian lu tng i ca acid
citric/acid tartric khong2,3.
Lp li cch tin hnh c m t trn trong phn Dn
xut ho v Sc k kh s dng 1 ml dung dch i chng
acid citric (3 mg/ml trong nc) thay th 1 ml dung dch mu
th.
Tnh kt qu:
o din tch mi pic bng phng php thch hp.
Acid citric tng (%) =
Trong :
ACS: Din tch pic ca acid citric (dung dch mu)
ATS: Din tch pic ca acid tartric (dung dch mu)
ATR: Din tch pic ca acid tartric (dung dch i chng)
ACR: Din tch pic ca acid citric (dung dch i chng)
WCR: Khi lng (g) ca acid citric trong 1 ml dung dch i
chng
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QCVN 4-22: 2011/BYT
Acid bo tng s
W: Khi lng (g) ca mu ester glycerol vi acid citric v

acid bo.
Cn chnh xc 5 g mu cho vo bnh y trn dung tch 250
ml, thm vo 50 ml dung dch KOH 1 N trong ethanol, v
un si vi ng sinh hn ngc trn ni cch thy trong 1
gi.
Chuyn ton lng dung dch trong bnh x phng ho vo
phu chit dung tch 1.000 ml, cho 3 ln 25 ml nc v
thm 5 git da cam methyl TS.
Thm cn thn dung dch HCl m c cho n khi mu
ca dung dch chuyn sang mu r rt v lc u tch
cc acid bo.
Trch ly cc acid bo tch c bng ba ln 100 ml dung
mi diethyl ether. Ho chung cc phn tch c v ra
mi ln bng 50 ml dung dch NaCl 10% cho n khi dung
dch NaCl c ra tr nn trung tnh.
Lm kh dung dch ether bng Na 2SO4 khan. Sau c bc
hi trn cch thy ether, thm 10 pht na trn cch
thy v cn phn cn.
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QCVN 4-22: 2011/BYT

Ph lc 4
I VI ESTER CA GLYCEROL VI ACID DIACETYL TARTRIC
V ACID BO
1. Tn khc, ch s
Diacetyltartric acid esters of mono- and diglycerides,

DATEM;
INS 472e
Tartric, acetic and fatty acid esters of glycerol, mixed; Mixed
acetic and tartric acid esters of mono and diglycerides of
fatty acids;
INS 472f
2. nh ngha
Sn phm gm hn hp cc ester ca glycerol vi acid

mono, diacetyltartric v cc acid bo thc phm. N c
tng hp bng phn ng gia anhydrid diacetyltartric v
mono, diglycerid ca acid bo c mt acid acetic, hoc
bng cch tng tc gia anhydrid acetic v mono,
diglycerid ca acid bo c mt acid tartric.
Do trao i nhm acyl trong ni phn t hoc gia cc phn
t, c hai phng php sn xut u to ra cc thnh phn
chnh nh nhau, vic to ra cc thnh phn chnh ph thuc
vo t l tng i ca cc nguyn liu c bn, vo nhit
v thi gian phn ng. Sn phm ny c th cha mt
lng nh glycerol t do, cc acid bo t do, acid tartric v
acid acetic t do. Sn phm thng mi c th c quy
nh cc ch tiu k thut r hn nh ch s acid, hm lng
acid tartric tng s, hm lng acid acetic t do, ch s x
phng ho, ch s iod, hm lng acid bo t do, im
ng c ca acid bo t do.
Cng thc cu to
Cc thnh phn chnh l:
Trong :
1) Mt hoc hai nhm R l ca acid bo
2) Nhm R khc l ca hoc
- acid diacetylat tartric
- acid monoacetylat tartric
- acid tartric
- acid acetic
- hydrogen
3. Cm quan
T dng lng, bt nho n dng rn ging sp (vy hoc

bt)
4. Chc nng
Cht nh ho
5. Yu cu k thut
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QCVN 4-22: 2011/BYT

5.1. nh tnh
tan
Phn tn trong nc nng v nc lnh, tan trong methanol

v ethanol.
1, 2- diol
Phi c phn ng c trng ca 1,2-diol.
Acid bo
Phi c phn ng c trng ca acid bo
Acid acetic
Phi c phn ng c trng ca acid acetic
Acid tartric
Phi c phn ng c trng ca acid tartric
Glycerol
Phi c phn ng c trng ca glycerol
5.2. tinh khit

Acid
Khng pht hin c cc loi acid khc ngoi acid acetic,

acid tartric v acid bo.
Tro sulfat
Khng c qu 0,5% c xc nh 800 25C
Acid bo t do
Khng c qu 3% tnh theo acid oleic
Acid acetic tng s
Khng c nh hn 8% v khng c qu 32% sau khi

thu phn (m t trong phn Phng php th)
Acid tartric tng s

x phng ho (m t trong phn Phng php th)
Glycerol tng s

x phng ho (m t trong phn Phng php th)
Glycerol t do
Khng c qu 2,0%
Ch
6. Phng php th
6.1. nh tnh
1, 2- diol
Cho vi git ch acetat TS vo dung dch c 500 mg mu

trong 10 ml methanol. Cht kt ta vn, mu trng khng
tan c hnh thnh.
6.2. tinh khit
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QCVN 4-22: 2011/BYT

Acid acetic tng s
Dng c:
Lp rp b dng c chng ct Hortvet Sellier ci tin nh
hnh v sau, s dng ng Sellier c kch thc bn trong
ln (khong 38-x 203 mm) v by chng ct dung tch ln.
Cch tin hnh:
Cn chnh xc 4 g mu v cho vo ng bn trong ca b
dng c v lp ng vo bnh ngoi c cha khong 300 ml
nc nng va un si. Thm 10 ml acid perchloric 4 N [35
ml (60 g) acid perchloric 70% trong 100 ml nc] vo mu
th, v ni ng bn trong vi sinh hn lm mt bng nc
qua by chng ct. Chng ct bng cch gia nhit bnh
pha ngoi sao cho thu c 100 ml dung dch ct trong
khong 20 - 25 pht. Tp hp cc phn dch ct c 100
ml v thm phenolphthalein TS vo mi phn, chun
bng dung dch NaOH 0,5 N. Tip tc chng ct cho n khi
phn 100 ml dung dch ct c cn khng qu 0,5 ml dung
dch NaOH 0,5N trung ho. (Ch : khng c chng
ct n cn kh). Tnh khi lng (mg) acid bay hi trong
mu theo cng thc V x e, trong V l tng th tch (ml)
ca dung dch NaOH 0,5N dng chun v e l h
s ng lng 30,03.
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QCVN 4-22: 2011/BYT

Acid tartric tng s
ng chun:
Chuyn 100 mg acid tartric tinh khit c cn chnh xc
vo bnh nh mc dung tch 100 ml, ho tan acid tartric
trong 90 ml nc v thm nc n th tch 100 ml, lc
u. Ly cc phn 3, 4, 5 v 6 ml cho vo cc cuvet ring
bit ph hp (kch thc 19 x 150 mm), thm lng nc
thch hp c dung dch th tch 10 ml. Cho vo mi
cuvet 4 ml dung dch natri metavanadat 5% va mi pha, 1
ml acid acetic. (Ch : s dng cc dung dch ny trong
vng 10 pht sau khi mu tng ln). Chun b mu trng
ging nh cch trn, s dng 10 ml nc thay th dung
dch acid tartric. t thit b v tr bng 0 i vi mu trng
v sau o hp th ca 4 dung dch acid tartric ti
bc sng 520 nm vi my quang ph thch hp hoc my
so mu quang in c trang b knh lc 520 nm. T s
liu thu c, xy dng ng chun trn h trc to
vung gc vi trc tung biu din hp th, trc honh
biu din lng acid tartric tng ng (mg).
Chun b mu th:
Cn chnh xc 4 g mu cho vo bnh tam gic dung tch 250
ml, thm vo 80 ml dung dch KOH 0,5N v 0,5 ml
phenolphthalein TS. Ni bnh vi mt sinh hn khng kh c
chiu di t nht 65 cm, gia nhit hn hp trn tm nhit
trong 2,5 gi. Thm vo hn hp nng khong 10% acid
phosphoric cho n khi hn hp c phn ng acid r vi
giy ch th Congo. Ni li bnh vi sinh hn khng kh v
gia nhit cho n khi acid bo c ho lng v trong. Lm
ngui v sau chuyn hn hp vo mt bnh gn dung
tch 250 ml vi s h tr ca cc phn nh nc v
chloroform. Chit cc acid bo c gii phng ra bng 3
ln 25 ml nc ct lin tip v cho phn nc ra vo bnh
gn c cha lp nc. Chuyn ton b hn hp trong bnh
gn u vo cc dung tch 250 ml, gia nhit trn ni cch
thy loi b cc vt ca chloroform, lc qua giy lc mn
c ra acid vo bnh nh mc dung tch 500 ml, v
cui cng pha ti th tch 500 ml bng nc ct (Dung dch
I). Dng pipet ly 25 ml dung dch ny cho vo bnh nh
mc dung tch 100 ml v pha ti th tch 100 ml bng nc
(Dung dch II). Gi phn cn li ca Dung dch I xc nh
glycerol tng s.
Cch tin hnh:
Cho 10 ml Dung dch II c chun b trong phn Chun
b mu th vo cuvet 19 x 150 mm v tip tc lm theo
hng dn trong phn ng chun, bt u vi cho vo
mi cuvet 4 ml dung dch metavanadat 5%. T ng
chun xc nh khi lng (mg) acid tartric trong ln pha
long cui cng, sau nhn vi 20 v chia kt qu cho
khi lng mu gc thu c % acid tartric.
Glycerol tng s
Chuyn 5 ml Dung dch I chun b trong phn xc nh

15
QCVN 4-22: 2011/BYT

Acid tartric tng s vo trong bnh bnh tm gic c np thu
tinh dung tch 250 ml hoc bnh iod. Thm vo bnh 15 ml
acid acetic bng v 25 ml dung dch acid periodic, c
chun b bng cch ho tan 2,7 g acid periodic (H 5IO6) trong
50 ml nc, thm 950 ml acid acetic bng v lc mnh; bo
qun dung dch ny trnh nh sng. Lc u hn hp trong
1 hoc 2 pht, yn trong 15 pht, thm 15 ml dung dch
KI 15% v 15 ml nc, lc xoy, yn trong 1 pht v sau
chun iod c gii phng ra bng dung dch natri
thiosulfat 0,1N, dng tinh bt TS l cht ch th. Thc hin
chun mu trng s dng nc thay th mu th. Th
tch thc l s ml dung dch natri thiosulfat 0,1N dng
chun glycerol v acid tartric trong mu th c 5 ml Dung
dch I. T % xc nh c trong Phng php th Acid
tartric tnh th tch dung dch natri thiosulfat 0,1N dng
chun acid tartric. Chnh lch gia th tch thc v th
tch tnh ton c dng i vi acid tartric l s ml ca
dung dch natri thiosulfat 0,1N tiu th bi glycerol trong
mu. Mt ml dung dch natri thiosulfat 0,1N tng ng
vi 2,303 mg glycerol v 7,505 mg acid tartric.
Dng c chng ct Hortvet-Sellier ci tin

Ch

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.
16
QCVN 4-22: 2011/BYT

Ph lc 5
YU CU K THUT V PHNG PHP TH I VI SUCROGLYCERID
1. Tn khc, ch s
2. nh ngha
INS 474
Sucroglycerid thu c nh phn ng gia sucrose
vi cht bo hoc du n c hoc khng c mt ca
dung mi. Sn phm gm c hn hp mono- v diester ca sucrose v acid bo kt hp vi mono-, div triglycerid t cht bo hoc du. Ch cc dung
mi sau y c th c s dng trong sn xut:
dimethyl formamid, cyclohexan, isobutanol, isopropanol v
ethyl acetat.
3. Cm quan
Khng mi, dng mm, dng c, dng bt c mu trng

n trng nht, hoc dng gel cng.
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc lnh, tan trong ethanol.
Acid bo
ng
Phi c phn ng c trng ca ng.
5.2. tinh khit

Tro sulfat
Khng c qu 2%
Th 2 g mu (Phng php I)
Ch s acid
Khng c qu 6
Sucrose t do
Khng c qu 5% (m t trong phn Phng php th)
Dimethylformamid
Khng c qu 1 mg/kg (m t trong phn Phng php

th)
Cyclohexan v
isobutanol
Khng c qu 10 mg/kg, dng n cht hoc hp

cht (m t trong phn Phng php th)
Ethyl acetat v
isopropanol
Khng c qu 350 mg/kg, dng n cht hoc hp cht
Ch
5.3. Hm lng
Khng c nh hn 40% v khng c ln hn 60%

ester sucrose
6. Phng php th
6.1. nh tnh
Acid bo
Cho 1 ml ethanol vo 0,1 g mu, lm m v ho tan, thm

5 ml dung dch H2SO4 long TS, gia nhit trong ni cch
17
QCVN 4-22: 2011/BYT

thy trong 30 pht v lm ngui. Cht c mu trng vng
hoc du c hnh thnh, v c ho tan khi thm 3 ml
diethyl ether.
18
QCVN 4-22: 2011/BYT

ng
Cho vo 2 ml lp dung dch nc tch ra t cht c hoc

du trong php th acid bo, 1 ml anthron TS vo trong
ng th, cho chy cn thn vo thnh ng th; b mt
ranh gii gia hai lp chuyn thnh mu xanh da tri hoc
xanh l cy.
6.2. tinh khit

Sucrose t do
Xc nh bng sc k kh lng (xem Quyn 4)

Ho cht, thuc th:
- Dung dch ni chun: Dung dch cholesterol trong
chloroform 5 mg/ml hoc tetracosan trong chloroform 10
mg/ml
- Pyridin (lm kh c qua ry phn t)
- N, O- Bis-(trimethylsilyl)-acetamid (BSA)
- Trimethylchlorosilan (TMCS)
Cch tin hnh: Cn chnh xc 20 50 mg mu cho vo
bnh silyl ha, thm 1 ml dung dch ni chun, 1 ml pyridin,
0,5 ml N, O-bis (trimethylsilyl) acetamid (BSA) v 0,5 ml
trimethylchlorosilan (TMCS). y np bnh v gia nhit
700C trong 30 pht. Bm 1l vo thit b sc k kh lng.
Cc iu kin sc k:
Ct:
- Chiu di 0,3 m
- ng knh trong 4 mm
- Cht liu: thu tinh
- c nhi bng dexil
Kh mang: nitrogen
Tc dng: 40 ml/pht
Detector: FID
Chng trnh nhit : gi 160 0C trong 1 pht sau
tng n 160 3750C vi tc 150C/pht.
o cc din tch pic ca sucrose v ni chun. H s p
ng (RF) c tnh t qu trnh chy sc k kh lng vi
cc
dung dch chun sucrose cha ni chun.
Kt qu:
mg ni chun x din tch pic sucrose
RF = ----------------------------------------------------Din tch pic ni chun x mg sucrose
v
mg ni chun x din tch pic sucrose x
100
% sucrose t do =
--------------------------------------------------------19
QCVN 4-22: 2011/BYT

RF x din tch ni chun x mg mu
20
QCVN 4-22: 2011/BYT

Dimethylformamid
Xc nh bng sc k kh lng
Ho cht, thuc th:
- Dimethyl formamid
- Dimethylamin hydrochlorid
- Methanol
- Ethanol
- HCl
- NaOH
Dung dch chun:
Chun b dung dch gc dimethylaminhydroclorid trong
ethanol 4,47 mg/ml (tng ng vi 4,0 mg/ml dimethyl
formamid) v chun b mt lot cc dung dch chun tng
ng vi 4; 2 v 1 g/ml dimethylformamid bng cch pha
long dung dch gc vi dung dch NaOH 0,1% trong
ethanol.
Chun b mu:
B dng c thu phn c trnh by trong phn Ph lc.
Cn chnh xc 40 g mu cho vo bnh y trn dung tch
1.000 ml. Thm 500 ml dung dch NaOH 5% trong
methanol, v gn bnh vo b dng c thu phn. t bnh
ct bnh tam gic cha 10 ml dung dch HCl 1% trong
methanol vo b dng c thu phn. Gia nhit bnh y
trn v chng ct vi sinh hn ngc c nc lm mt
trong 1 gi, sau ct ly 50 ml dch ct c th dng li.
C dch ct c cho n kh trong cch thy si. Ho tan
phn cn bng mt lng nh ethanol, thm 2,5 ml dung
dch NaOH 5% trong ethanol v pha long n th tch 25
ml bng ethanol chun b mt dung dch mu.
Cch tin hnh:
Bm 2 l dung dch mu vo thit b sc k kh lng vi
cc iu kin di y.
ng chun:
Chun b ng chun bng cch bm 2 l cc dung dch
chun vo thit b sc k kh.
Cc iu kin sc k:
Ct:
- Di: 2m
- ng knh trong: 2 mm
- Cht liu: thu tinh
- Ct nhi: 10% amin 220 v KOH 10% trn nn
chromosorb W yu 80/100 c ra acid yu
- Luyn ct: Gia nhit ti 130 0C qua m vi tc dng
nitrogen 5 ml/pht
Kh mang: nitrogen
21
QCVN 4-22: 2011/BYT

Tc dng: 17 ml/pht
Detector: FID
Nhit :
- Bung bm mu: 198 50C
- Ct: 600C.
Tnh kt qu:
Nng dimethylformamid (CDFA) tnh theo cng thc sau:
Trong :
C: Nng dimethylformamid pht hin c (g/ml)
W: Khi lng mu (g)
22
QCVN 4-22: 2011/BYT

Cyclohexan v
isobutanol
Xc nh bng sc k kh lng (xem Quyn 4) s dng cc

iu kin sau:
Ho cht, thuc th:
- Dimethylformamid (tinh khit dng cho GLC)
- Cyclohexan (dng cho quang ph UV)
- Isobutanol (dng cho phn tch)
Dung dch chun:
Chun b dung dch gc cyclohexan v isobutanol trong
dimethylformamid bng cch dng pipet ly 130 l
cyclohexan v 125 l isobutanol cho vo dimethylformamid
v lm y n th tch 10 ml.
T dung dch gc trn pha mt lot cc dung dch chun
pha long c 5, 10 v 20 mg/kg cyclohexan v isobutanol.
V ng p ng bng cch bm 5 l cc dung dch
chun pha long vo thit b sc k kh vi cc iu
kin sau.
Chun b mu th:
Cn 5 g mu chnh xc n 10 mg cho vo bnh c np
y thu tinh, thm vo 5 g dimethylformamid v lm m
ho tan. Lm ngui v bm 5 l vo thit b sc k kh
vi cc iu kin sau.
Ct:
- Di: 3m
- ng knh trong: 4,5 mm
- Cht liu: thp khng r
- Cht nhi: 20% carbowax 20 M trn Chromosorb G 60/80
Kh mang: heli (p sut 1,6 bar)
Detector: ion ho ngn la
Nhit :
- Bung bm mu: 1300C
- Ct: 1300C
- Detector: 2000C
Xc nh nng cyclohexan v isobutanol trong dung
dch mu (50%) bng cch so snh vi cc dung dch
chun v nhn nng vi 2 chuyn cc kt qu cho
ph hp vi sucroglycerid gc.
23
QCVN 4-22: 2011/BYT

Isopropanol v ethyl
acetat
Xc nh bng sc k kh (xem Quyn 4) c bung ly mu

khng gian hi s dng cc iu kin sau:
Ho cht, thuc th:
- Isopropanol
- Ethyl acetat
Dung dch chun:
Ly 1 g mi loi isopropanol v ethyl acetat vo mt bnh
nh mc v thm nc cho n khi t th tch 100 ml, v
pha long dung dch ny c cc dung dch c nng
0,02 0,4 g/100 ml.
Nu cn, chun b cc dung dch chun cha ti 7 g/100
ml isopropanol v ethyl acetat.
Cch tin hnh:
Cn 1 g chnh xc n 0,1 g bt mu cho vo l mu.
Thm 5 l nc vo l mu v np kn nhanh bng
septum. l mu vo thit b sc k kh t trc
chng trnh v bt u phn tch theo cc iu kin
cp di y.
ng chun:
Ly 1 g bt ester ca sucrose vi cc acid bo, khng
cha dung mi hoc cc dung mi tn d bit, cho vo
l mu, thm 5 l dung dch chun v y kn bng
septum. l mu vo thit b sc k kh t trc
chng trnh v bt u phn tch theo cc iu kin
cp di y v v c ng chun ca mi dung mi.
Ct:
- Di: 30 m
- ng knh trong: 0,53 mm
- Cht liu: mao qun silica
- Fim mng: 100% methyl polysiloxan
- Luyn ct: Gia nhit ti 60 0C trong 2 3 gi vi tc
kh nitrogen khong 10 ml/pht.
Kh mang: nitrogen
Tc dng: 5 ml/pht
Detector: ion ho ngn la
Nhit :
- Bung bm mu: 1100C
- Ct: 400C.
- Detector: 1100C
Bung khng gian hi:
- Lng mu: 1 g 0,1 g + 5 l
- Nhit gia nhit mu: 800C
- Thi gian gia nhit mu: 40 pht
24
QCVN 4-22: 2011/BYT

- Nhit syringe: 850C
- Th tch mu dng hi: 0,4 ml
Kt qu: c tnh theo cng thc:
Trong :
Ci: Nng dung mi i (mg/kg);
Ai: Din tch pic dung mi i (v.giy.);
Cfi: H s chuyn i dung mi i ( dc ca ng
chun) (g/v.giy).
25
QCVN 4-22: 2011/BYT

Ch

- 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.
6.2. nh lng
Xc nh bng sc k lng cao p (xem Quyn 4) s dng

cc iu kin sau:
Chun b mu:
Cn chnh xc 250 mg mu cho vo bnh nh mc 50 ml.
Pha ti th tch 50 ml bng tetrahydrofuran v lc u. Lc
qua mng lc 0,5 m.
Cch tin hnh:
Bm 100 l mu vo thit b sc k lng cao p n nh
trc.
Cc iu kin sc k:
Ct: Styren-divinylbenzen copolymer i vi sc k thm
thu qua gel (TSK-GEL G2000 (Supelco) hoc tng
ng)
Pha ng: tetrahydrofuran dng cho HPLC ui kh
Tc dng: 0,7 ml/pht
Detector: RI (ch s khc x)
Nhit :
- Ct: 380C.
- Detector: 380C
Ghi sc k trong khong 90 pht.
Tnh % ester sucrose trong mu:
% ester sucrose = 100 A/T
Trong :
A: Tng cc din tch pic i vi 3 thnh phn chnh,
mono-, di- v tri-ester, ra gii ln lt khong 65, 68 v
73 pht.
T: Tng din tch tt c cc pic ra gii trong khong 90
pht
Ph lc:
26
QCVN 4-22: 2011/BYT
B dng c thu phn:

a: Sinh hn ngc
b: SInh hn
c: Bnh y trn
d: Chu nc
e: Bnh tam gic
27
QCVN 4-22: 2011/BYT

Ph lc 6
YU CU K THUT V PHNG PHP TH I VI ESTER CA
POLYGLYCEROL VI CC ACID BO
1. Tn khc, ch s
2. nh ngha
Polyglycerol fatty acid esters, glyceryl fatty acid esters;

INS 475
L cc ester mt phn hn hp c to thnh bng phn
ng glycerol polymer ha vi m v du n, hoc vi
acid bo; c th cha mt lng nh mono-, di- v
triglyceride, glycerol t do v polyglycerol, acid bo t do
v mui natri ca cc acid bo; polymer ha c th thay
i v c ch ra bng mt con s (th d l tri-, 3), l
s trung bnh nhm (gc) glycerol tnh cho 1 phn t
polyglycerol. Mt polyglycerol nht nh bao gm mt s
phn b cc mnh phn t c trng cho polymer ha
danh nh ca n. Bng cch thay i t l cng nh bn
cht cc cht bo hoc acid bo phn ng vi
polyglycerol, ngi ta thu c mt nhm ln v a dng
cc sn phm ester ny;
Cc sn phm ester thng mi cn c c trng vi 1
s ch tiu khc nh ch s x phng ha, im ng c
ca acid bo t do, ch s iod, ch s hydroxyl v hm
lng tro.
Cng thc cu to
Trong gi tr trung bnh ca n khong l 3 v mi R 1, R2,

R3 c th l ca acid bo hoc hydro.
3. Cm quan
Dng lng nh du ti rt nht, c mu vng sng n h

phch; cht do hoc nha c mu vng nht n mu
nu; cht rn hoc cht sp c mu vng nht n mu
nu.
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
T rt a nc ti rt a du, nhng l mt loi cht c

xu hng phn tn trong nc v ha tan trong dung mi
hu c v cc loi du.
Acid bo
Glycerol v polyglycerol
Phi c phn ng c trng ca glycerol v polyglycerol.
5.2. tinh khit

Acid
Khng pht hin c acid no ngoi acid bo.
Polyglycerol
Phn polyglycerol gm c khng nh hn 70% di-, tri-,

tetraglycerol v phi c khng qu 10% polyglycerol bng
28
QCVN 4-22: 2011/BYT

hoc cao hn heptaglycerol.
Ch
6. Phng php th
6.1. nh tnh
Glycerol v polyglycerol
Chm 5 20 l lp dung dch nc thu c trong php

th acid bo Php th nh tnh cc nhm chc dc theo
cc chm i chng glycerol trn giy Whatman s 3 v
trin khai sc k i xung trong 36 gi vi h dung mi
isopropanol: nc (90:10 ). Vt glycerol di chuyn c
40 cm v tip sau l cc polyglycerol c pht hin ln
lt pha di sau glycerol khi giy c phun hoc
permanganat trong aceton hoc bc nitrat trong amoniac.
6.2. tinh khit

Ch

29
QCVN 4-22: 2011/BYT

Ph lc 7
YU CU K THUT V PHNG PHP TH I VI STEARYL CITRAT
1. Tn khc, ch s
INS 484
ADI = 0 - 50 mg/kg th trng, c thit lp ti k hp ln
th 17 ca JECFA (1973).
2. nh ngha
c tng hp bng cch ester ha acid citric vi cn

stearylic thng mi, c th cha n-octadecanol v n
50% n-hexadecanol v t c cc yu cu di y.
Ch phm thng mi c th c phn loi theo ch s x
phng ha; hm lng v thnh phn ca cn stearylic; ch
s iod; ch s acid v hm lng acid citric.
Cng thc cu to
Thnh phn gn ng
Trong R1, R2 v R3 ln lt c th l C18H37 (stearyl),

C16H33 (palmityl) hoc H
3. M t
Hp cht nhn, mu kem.
4. Chc nng
Cht to phc kim loi, cht nh ha.
5. Tnh cht
5.1. nh tnh
tan
Khng tan trong nc v trong ethanol lnh, tan trong

ethanol nng.
Cn stearylic
Phi c phn ng c trng ca cn stearylic.
Citrat
Phi c phn ng c trng ca citrat.
5.2. tinh khit

Cc acid khc v ru
khc
Khng c c cc acid khc ngoi acid citric v cc ru

khc ngoi cc ru c mt trong ch phm cn stearylic
thng mi.
Cht khng tan trong

cloroform
Khng c qu 0,5% (m t trong phn Phng php

th).
Ch
6. Phng php th
6.1. nh tnh
Cn stearylic
Thy phn 2 g mu th bng cch un hi lu trong 1 gi

vi 50 ml dung dch natri hydroxyd (TS) thu c dung dch
nc. Lm mt v chit vi ether du ha. Ly lp ether
30
QCVN 4-22: 2011/BYT

du ha v cho bay hi trn a s hoc thy tinh. Phn
khng bay hi phi c khong nng chy t 43 o n 58o.
Citrat
Ly 5 ml dung dch nc thu c trong php th cn

stearylic, thm 1 ml dung dch calci clorid (TS) v 3 git
dung dch xanh da tri bromothymol (TS), acid ha nh
bng dung dch acid hydrocloric long (TS). Thm dung
dch natri hydroxyd (TS) n khi dung dch chuyn thnh
mu xanh da tri sng, sau un si dung dch trong 3
pht, lc nh trong khi un. Trong dung dch xut hin kt
ta trng, kt ta ny khng tan trong dung dch natri
hydroxyd (TS) nhng tan trong dung dch acid acetic (TS).
Ly 10 ml dung dch nc thu c trong php th cn
stearylic, thm 1 ml dung dch thy ngn (II) sulfat (TS).
un si hn hp v thm vi git dung dch kali
permanganat (TS). Trong dung dch xut hin kt ta trng
l mui thy ngn ca acid aceton dicarboxylic.
6.2. tinh khit

Cht khng tan trong
cloroform
Ch
Ha tan khong 50g (cn chnh xc n mg) mu trong 400

ml cloroform. Lc dung dch qua phu lc thy tinh xp s 3
cn b (chnh xc n mg). Gi phu lc cn m, ra
phn khng tan bng cloroform, sau sy kh ti 100 o.
31
QCVN 4-22: 2011/BYT

Ph lc 8
I VI TRIKALI ortho-PHOSPHAT
1. Tn khc, ch s
Tripotassium phosphate; Tribasic potassium phosphate;

Potassium phosphate.
INS 340iii
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm
2. nh ngha
Tn ha hc
Trikali phosphat; Trikali orthophosphat; Trikali

monophosphat
Ch s C.A.S.
7778-53-2
Cng thc ha hc
Dng khan: K3PO4

Dng hydrat: K3PO4.xH2O
Khi lng phn t
212,27 (dng khan)
3. Cm quan
Dng tinh th hoc ht khng mu hoc mu trng, khng

mi; dng hydrat gm monohydrat v trihydrat
4. Chc nng
m, cht nh ha, cht to phc kim loi
5. Yu cu k thut
5.1. nh tnh
tan
D tan trong nc, khng tan trong ethanol.
pH
11,5 - 12,5 (dung dch 1/100).
Kali
Phi c phn ng c trng ca kali.
Phosphat
Phi c phn ng c trng ca phosphat.
ortho-phosphat
Phi c phn ng c trng ca ortho-phosphat.
5.2. tinh khit

o
Gim khi lng khi nung Dng khan: Khng c qu 3% (120 C trong 2 gi, sau
0
800 C trong 30 pht)
Dng hydrat: Khng c qu 23% (120 oC trong 2 gi, sau
800oC trong 30 pht)
Cc cht khng tan trong

nc
Khng c qu 0,2%.
Fluorid
Arsen
Khng c qu 3,0 mg/kg (th theo hng dn ti JECFA

monograph 1 - Vol.4 - phng php II).
Ch

32
QCVN 4-22: 2011/BYT

5.3. Hm lng K3PO4
Khng c thp hn 97,0% sau khi nung
6. Phng php th
6.1. nh tnh
Kali
Thm 1 th tch dung dch natri hydrogen tartrat bo ha v

1 th tch dung dch ethanol vo dung dch mu th (1/100)
v lc. Trong dung dch phi xut hin kt ta tinh th trng.
Phosphat
Thm 1ml dung dch acid nitric v 5ml dung dch nhm
molybdat (TS) vo 5ml dung dch mu th (1/100) v un
nng. Trong dung dch phi xut hin kt qu vng nht.
ortho-phosphat
Ha tan 0,1g mu th trong 10ml nc ct, acid ha nh

dung dch bng acid acetic long (TS) v thm 1ml bc
nitrat (TS). Trong dung dch phi xut hin kt ta mu
vng
6.2. tinh khit

Fluorid
Cn 5 g mu th cho vo mt bnh cu ct 250 ml, thm 25

ml nc, 50 ml acid percloric, 5 git dung dch bc nitrat (1
trong 2) v vi vin bi thy tinh. Ni bnh cu vi 1 sinh hn
c gn nhit k v mt ng mao qun sc kh, u nhit k
v ng mao qun phi ngp trong dung dch cha trong
bnh. Gn mt phu nh git cha nc hoc b sinh hi
nc vo ng mao qun. t bnh trn tm aming c l
sao cho 1/3 y bnh tip xc vi ngn la. Tin hnh ct
n khi nhit trong bnh t 135 o. Thm nc t phu
vo bnh hoc cho hi nc qua bnh duy tr nhit
trong bnh lun t 135o-140o. Tip tc ct n khi thu c
225-240 ml dch ct sau pha long dch ct thu c vi
nc n 250 ml, lc u. Ly 50 ml dung dch ny cho
vo mt ng Nessler 100 ml. Trong mt ng Nessler tng
t khc ly 50 ml lm mu chng. Thm vo mi ng 0,1
ml dung dch natri alizarinsulfonat (nng 1/4000) lc
v 1 ml dung dch hydroxylamin (nng 1/4000) mi pha,
lc u. Thm tng git dung dch natri hydroxyd 0,05 N
vo ng cha dch ct, va thm va khuy, n khi mu
ng cha dch ct ging vi mu ng chng l mu hng
nht. Sau thm vo mi ng ng chnh xc 1 ml dung
dch acid hydrocloric 0,1 N v lc u. S dng buret chia
vch 0,05 ml thm t t va dung dch thori nitrat (nng
1/4000) vo ng cha dch ct sau khi lc u mu
ca dung dch chuyn v mu hng nht. Ghi th tch dung
dch thori nitrat (nng 1/4000) s dng, thm chnh
xc lng dung dch thori nitrat (nng 1/4000) nh vy
vo ng chng, lc u. Dng buret thm dung dch natri
fluorid (TS) (10 g F / ml) vo ng chng cho mu hai
ng ging nhau sau khi pha long v cng th tch. Lc
u, yn cho bt kh thot ht trc khi so mu. Kim
tra im tng ng bng cch thm 1-2 git dung dch
natri fluorid (TS) vo ng chng. S thay i mu r rt s
xy ra. Ghi li th tch dung dch natri fluorid (TS) s
33
QCVN 4-22: 2011/BYT

dng.
Th tch dung dch natri fluorid (TS) s dng khng c
qu 1 ml.
Ch
6.3. nh lng
Cn mu th (chnh xc n mg), khi lng tng ng

vi 8g K3PO4 khan, ha tan vo trong 40 ml nc ct trong
cc 400ml. Thm 100ml dung dch acid hydrocloric 1N. Sc
khng kh kh carbon dioxyd vo dung dch, ch sao cho
bt kh nh, thi gian sc 30 pht ui ht carbon
dioxyd, y nh cc trnh mt dung dch trong khi sc.
Ra np v thnh cc bng nc ct v cho in cc ca
pH k thch hp vo dung dch. Chun dung dch bng
dung dch natri hydroxyd 1N n im un ti pH~4, sau
tnh th tch (A) dung dch acid hydrocloric 1N s dng.
Bo v dung dch trnh hp th carbon dioxyd t khng
kh v tip tc chun vi dung dch natri hydroxyd 1N
n im un ti pH~8,8. Tnh th tch (B) dung dch natri
hydroxyd 1N tiu tn trong chun ny.
Nu (A) 2(B), mi ml natri hydroxyd 1N trong th tch (B)
tng ng vi 212,3mg K3PO4.
Nu (A) < 2(B), mi ml natri hydroxyd 1N trong hiu th tch
(A)-(B) tng ng vi 212,3mg K3PO4.
Ph lc 9
I VI CC MUI AMONI CA ACID PHOSPHATIDIC
1. Tn khc, ch s
Ammonium phosphatides, Emulsifier YN, Mixed ammonium

salts of phosphorylated glycerides;
INS 442
ADI = 0 -30 mg/kg th trng
2. nh ngha
Ch phm ny ch yu gm hn hp cc hp cht amoni

ca cc acid phosphatidic bt ngun t cht bo n c
(thng l du ht ci hydrogen ha mt phn). L mt
mono- hoc diglycerid c th c gn phosphor. Tuy nhin,
hai ester phosphor c th lin kt vi nhau dng
phosphatidyl phosphatid. Ch phm c sn xut bng
cch phn hy cht bo bng glyceryl, sau phosphoryl
ha bng phosphor pentoxyd, v trung tnh ha bng
amoniac.
Ch phm thng mi c th c quy nh thm nhng chi
tit c th nh hm lng nc, tp cht khng tan trong
34
QCVN 4-22: 2011/BYT

hexan, cht v c khng tan trong hexan, gi tr pH v hm
lng triglycerid.
Cng thc cu to
(thnh phn gn ng)
Trong R c th l mt gc mono- hoc di-glycerid

3. Cm quan
Cht na rn trn nhn.
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, tan mt phn trong ethanol v aceton;

tan trong cht bo.
Phosphat
Acid bo
Glyceryl
Phi c phn ng c trng ca glyceryl.
5.2. tinh khit

Ch
5.3. Hm lng
Hm lng phosphor khng c nh hn 3,0% v khng

ln hn 3,4% theo khi lng; hm lng nitrogen amoni
khng c nh hn 1,2% v khng ln hn 1,5%.
6. Phng php th
6.1. nh tnh
Phosphat
Nung 1 g mu th vi 2 g natri carbonat khan. ngui v

ha tan cn trong 5 ml nc v 5 ml acid nitric. Thm 5 ml
amoni molybdat (TS) v un ti si. Xut hin kt ta mu
vng.
Acid bo
un hi lu 1 g ch phm th trong 1 gi vi 25 ml kali

hydroxyd 0,5 N trong ethanol. Amoniac bay ra t pha u
ca ng sinh hn hi lu, nhn ra bng mi ca n v phn
ng trn giy qu m. Lm lnh cn ti 0 oC, ta x phng
kali to thnh.
6.2. tinh khit

Ch

35
QCVN 4-22: 2011/BYT

6.3. nh lng
Phosphor
Phng php quang ph hp th

Thuc th v dung dch lm vic
Acid sulfuric: t trng tng i 1,84
Acid nitric: t trng tng i 1,42
Acid perchloric: 60%, t trng tng i 1,54
Dung dch vanadat-molybdat: Ha tan ring trong nc 20 g
amoni molybdat v 1 g amoni vanadat. Trn hai dung dch,
thm 140 ml acid nitric c v pha long ti 1000 ml bng
nc. Lc u.
Dung dch phosphat chun: Dung dch gc: Ha tan 3,8346 g
kali dihydro phosphat, lm kh 110C, vo trong nc
v pha long ti 1000 ml; 1 ml dung dch ny = 2,0 mg P 2O5.
Dung dch chun lm vic phosphat: Chuyn 50,0 ml dung
dch phosphat chun (1ml = 2,0 mg P2O5) vo bnh nh mc
500 ml v pha long ti vch bng nc v lc u. 1 ml
dung dch chun lm vic phosphat = 0,2 mg P2O5.
Tin hnh
Cn chnh xc 1,5 ti 1,6 g mu th vo mt bt thy tinh
nh v cho vo trong bnh Kjeldahl 300-ml cha 5 ml acid
sulfuric v 10 ml acid nitric. un nng bnh, u tin un nh
v lc lin tc, sau un mnh hn trn ngn la trn.
Thm nhiu ln ti cc thi im khc nhau mi ln mt
lng acid nitric, lm ngui bnh trc khi thm, v tip tc
un ti khi thu c dch phn hy trong v c mu vng
kim. ngui, thm 5 ml acid percloric 60% v tip tc oxy
ha ti khi to thnh khi acid trng trong bnh. Li lm ngui
v thm 5 ml nc v tip tc un ti khi ht khi trng bay
ln. ngui, pha long cn thn bng nc, li ngui v
chuyn ton lng sang bnh nh mc 500-ml. Pha long
ti vch bng nc v lc u (Dung dch th).
Lm mt mu trng phn hy ng theo cch nh trn
nhng khng cho mu th v s dng cng th tch acid nh
dng v c ha t mu th (Dung dch trng phn
hy).
Cho vo cc bnh nh mc 100-ml ring, thm t buret:
(a) 25,0 ml dung dch chun lm vic phosphat (= 5,0 mg
P2O5),
(b) 30,0 ml dung dch chun lm vic phosphat (= 6,0 mg
P2O5),
(c) 25 ml dung dch th cha t 5 n 6 mg P2O5
Cho vo mi bnh cha phosphor chun, (a) v (b), mt
lng dung dch trng phn hy c cng th tch nh dung
dch cho vo (c), b i vi vt phosphor c th c do
thuc th phn hy acid m n c th c trong dung dch
th.
Cho vo mi bnh 25 ml thuc th vanadat-molybdat, lc
u, pha long bng nc ti gn 100 ml, lc u, iu
chnh nhit ca dung dch ti 20C, pha long ti vch
bng nc v lc u.
Sau 10 pht, o hp th ca c dung dch 6 mg P 2O5 v
36
QCVN 4-22: 2011/BYT

dung dch th, mu trng l dung dch cha 5 mg cht
chun. Dng cc o 1 cm v o bc sng 420 nm, hoc
knh lc Ilford 604 nu dng my so mu quang in.
Tnh ton
A t 0,873
% phosphor 5

A 6mg
m
Trong :
At = hiu hp th gia chun 5 mg v dung dch th
A6 mg = hiu hp th gia chun 6 mg v 5 mg
m = khi lng mu th (g)
Thit b ct ko hi nc
Xc nh nitrogen amoni
Thit b gm mt bnh 2-L y nt cao su, lp xuyn qua nt
c mt ng thy tinh khong 7,5 cm, c lp sao cho u
di ca ng gn st y bnh, v mt on ng hnh ch L
ngn hn lp sao cho ng cha ngang khong 6 mm bn
di b mt ca nt, hot ng nh ng ra ca lung hi
nc. Bnh c thm nc ct acid ha nh bng acid
sulfuric long (TS) ti khong 2/3 th tch bnh v vi mnh
thy tinh xp trnh tro khi hn hp trong bnh si mnh.
Bnh ny dng lm ngun cung cp hi nc. C th lp mt
vi vo bnh nu mun d dng b sung nc vo bnh gia
cc ln xc nh.
ng ra ca hi c ni qua mt by ngng ti u vo ca
u ct hi, ni vo mt bnh cu y trn c ngn 1-L c
bnh c B34. u ct phi sao cho ng u vo ca hi gn
chm y bnh 1-L v u ra phi ni vi hai by trnh bn,
mt gn nh ca bnh 1-L v ci kia gn nh ca mt sinh
hn thng ng, ni c B19, ni vi u ct. Sinh hn thng
phi lp vi ng u ra ko di, chm ti y ca mt bnh
nn 500-ml.
Thuc th
Dung dch acid boric 2% (kl/tt) trong nc
Dung dch natri hydroxyd 40% (kl/tt) trong nc
Acid hydrocloric 0,02 N
Hn hp ch th: Trn 5,0 ml dung dch xanh lc bromocresol
0,1% (kl/tt) trong alcol v 2,0 ml dung dch methyl 0,1%
(kl/tt) trong alcol v pha long ti 30 ml bng alcol 95%.
Dch silicon 200/50 MS
Tin hnh
Lp v cho hi nc i qua thit b. Cn chnh xc khong
0,2 g mu th mui amoni ca acid phosphatidic trung tnh
vo trong mt l thy tinh nh (ng knh khong 18 mm,
su khong 12 mm). Chuyn l v mu th cn vo bnh
ct v thm khong 250 ml nc ct. Ni u ct v by
chng bn vi bnh ct v sinh hn ng, lp sinh hn sao
cho u ra ngp di b mt ca 10 ml acid boric 2% v 1
ml hn hp ch th ng trong bnh nn 500-ml.
Thm vo bnh ct qua phu gn bng mt ng cao su gn
vo ng dn hi nc vo, 75 ml natri hydroxyd 40%, v ra
vo trong bng nc ct. B phu v ni ng vo ca hi vi
ngun cung cp hi. (C th cho natri hydroxyd vo bnh qua
37
QCVN 4-22: 2011/BYT

phu c kha, lp vi bnh ct nu mun v ra pha trong
bng nc ct. Nu lm nh vy phi duy tr mt lp cht
lng trn phu trong sut qu trnh thm v ct). Ct ko
mnh bng hi nc hn hp trong bnh ct v thu ly 200
ml dch ct vo trong acid boric. Trong qu trnh ct khuy
nh bnh ct nu cn, trnh mu th b lng ng xung
quanh b mt pha trn ca bnh. Khi thu lng dch
ct theo yu cu, h thp bnh hng, ngng cung cp hi
nc v ra pha trong ca sinh hn v bn ngoi u pha
di vi mt lng nh nc ct, gp dch ra vo bnh
hng.
Chun hn hp trong bnh hng bng acid hydrocloric
0,02 N. Lm t nht mt mu trng tin hnh theo cng cch
nhng khng c mu th.
Trong qu trnh ct c th c bt xut hin ca hn hp trong
bnh ct. Nu c, thm 2 git dch silicon vo bnh ct ti thi
im cho mu th; v mt lng tng t c cho vo
mu trng.
Tnh ton
Mi ml HCl 0,02 N = 0,2802 mg nitrogen.
Vt V o
28,02
% Nitrogen
mt
Trong
Vt = th tch dung dch HCl 0,02 N dng chun mu th
(ml)
Vo = th tch dung dch HCl 0,02 N dng chun mu trng
(ml)
mt = khi lng mu th (mg).
Ph lc 10
I VI SUCROSE ACETAT ISOBUTYRAT
1. Tn khc, ch s
SAIB
INS 444
2. nh ngha
Hn hp c to thnh bng cch este ha sucrose thc

phm vi anhydrid acetic v anhydrid isobutyric v chng
ct. Hn hp bao gm tt c cc este vi t l phn t ca
acetat v isobutyrat l khong 2:6
Tn ha hc
Sucrose diacetat hexaisobutyrat
Ch s C.A.S
137204-24-1; 27216-37-1; 126-13-6
Cng thc ha hc
C40H62O19 i vi sucrose diacetat hexaisobutyrat
38
QCVN 4-22: 2011/BYT

Cng thc cu to
Trong
R1 = -CH2OCOCH3
R2 = -CH2OCOCH(CH3)2, hoc -OCOCH(CH3)2
Khi lng phn t
832 856
C40H62O19 = 846,9
3. Cm quan
Dng lng mu vng nht, khng cn v c mi nh
4. Chc nng
Cht nh ha, cht iu chnh m c, cht to c i

vi ung khng cn
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, tan trong hu ht dung mi hu c.
Ch s khc x
n (40, D): 1,4492 1,4504
Khi lng ring
d (25, 25): 1,141 1,151
Hp th hng ngoi
Ph hng ngoi ca mu th phn tn trong kali bromid

tng ng vi ph hng ngoi chun trong Ph lc.
5.2. tinh khit

Ch s acid
Khng c qu 0,2 (s dng 50 g mu th).
Ch s x phng ha
Gia 524 v 540 (s dng 1 g mu th)
Triacetin
Khng c qu 0,1%.
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng
C40H62O19
Khng c nh hn 98,8% v khng c qu 101,9%.
6. Phng php th
6.1. tinh khit
Triacetin
S dng phng php sc k kh nh sau:

Dng c, thit b:
My sc k kh c trang b detector ion ha ngn la
Ct: thp khng r, di 1,5 m, ng knh trong l 3,2 mm.
Chun b mu:
39
QCVN 4-22: 2011/BYT

Pha long mu th bng cch cho thm mt th tch carbon
disulfid tng ng.
iu kin:
Pha tnh: SE-30, 3%
Pha rn: Chromosorb AW-DMCS, 80-100 mesh
Kh mang: Heli
Tc kh: 20 ml/min
Nhit
- Ct: Chng trnh nhit : ngay sau khi bm mu, nhit
ct tng t 1000 (ln n 3000C, tc tng 100C/pht.
- Nhit bung bm: 3000C
Th tch bm mu: 1 l
Ch

6.2. nh lng
S dng ch s x phng ha, tnh % C 40H62O19 theo cng
thc:
Trong
SV = ch s x phng ha
Ph hng ngoi
Sucrose acetat isobutyrat
40
QCVN 4-22: 2011/BYT

Ph lc 11
I VI ESTER CA GLYCEROL VI NHA CY
1. Tn khc, ch s
Ester gum;
INS 445
2. nh ngha
Ester phc hp ca triglycerol v diglycerol vi cc acid t

nha g thng thu c nh qu trnh trch ly gc cy
thng lu nm bng dung mi sau c tinh ch trong
h dung mi lng-lng. Loi tr khi cc yu cu k thut
ny l cc dn xut ca gum nha, dch tit ra t cy
thng sng, nha du thng cao v sn phm ph ca qu
trnh sn xut bt giy. Sn phm cui cng gm c 90%
acid nha v 10% cht trung tnh (cht khng acid). Phn
acid nha l mt phc hp ca cc ng phn acid
monocarboxylic diterpenoid c cng thc thc nghim in
hnh l C20H30O2, trong thnh phn chnh l acid abietic.
Glycerol ester ca nha g thng c tinh ch bng
phng php bc hi nc hoc chng ct ngc dng.
M s C.A.S.
8050-30-4
3. Cm quan
Cht rn mu vng n mu h phch nht
4. Chc nng
Thnh phn base trong ko cao su, cht nh ho, cht n

nh, cht n, cht iu chnh hng liu trong ung
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, tan trong aceton
Hp th hng ngoi
Ph hng ngoi ca lp mng mu c t trn tm kali

bromid tng ng vi ph hng ngoi in hnh di y
Alcol nha v glycerol

nha
Phi c phn ng c trng ca alcol nha v glycerol

nha.
5.2. tinh khit

Khng c mt nha du
cao (Lu hunh)
t yu cu (m t trong phn phng php th).
T trng
d (20, 25) : Khng c nh hn 0,935 khi xc nh trong

dung dch 50% trong d-limonen (97%, im si 175,5 176,00C, d (20, 4) : 0,84)
im nng chy
82 900C (m tr trong phn Phng php th)
Ch s acid
39
Ch s hydroxyl
15 45 (m tr trong phn Phng php th )
Ch

41
QCVN 4-22: 2011/BYT

6. Phng php th
6.1. nh tnh
Alcol nha v
glycerol nha
Cc nhm ester phc tp trong ester ca glycerol nha g

thng c kh bng phn ng vi mt hydrid kim loi
(natri bis (2-methoxy-ethoxy) nhm dihydrid) trong dung
dch toluen to thnh mt hn hp ca alcol nha v
glycerol nha. Cht kh d sau c thu phn bng
dung dch acid to thnh hai pha. Sc k kh ca pha
toluen to ra mt sc k ca alcol nha cu thnh ester
nha g thng v c th phn bit vi cc ester gum v
ester nha du cao. Nha g c th phn bit c vi
nha du cao da vo t l ca abietyl v dehydroabietyl
alcol: trong nha g abietyl chim u th, trong khi nha
du cao, dehydroabietyl chim u th. Nha g c th
phn bit c vi gum rosin da vo t l ca isopimaryl
v palustryl alcol: trong nha g isopimaryl chim u th,
trong khi gum rosin, palustryl chim u th. Sc k ca pha
trung tnh trong nc trn ct khc kim tra s xut hin
ca glycerol.
Thit b, dng c:
- Sc k kh c trang b detector ion ho ngn la
- Ct sc k I: Column I: DB-1 methyl silicon (ngoi quan
v lin kt cho), ct mao qun di 15 m, ng knh trong
0,53 mm, dy 1,5 m, di nhit 60 - 300/3200C (V d: J
& W Scientific Inc,. Cat. No. 125-1012). C ng dn
bm hi nhanh, trc tip.
- Ct sc k II: : DB-Wax polyethyleneglycol (ngoi quan v
lin kt cho), ct mao qun di 15 m, ng knh trong
0,53 mm, dy 1,0 m, di nhit 20 - 2300C (V d: J & W
Scientific Inc,. Cat. No. 125-7012).
- B ghi: 0 1V
- Syringe: 1 l
- Pipet: 3,0 ml; 5,0 ml
- Bnh tam gic: 25 ml
- L: 17 ml
- Cn phn tch: cn chnh xc n 0,001 g
- ng li tm c vch nh mc: 15 ml
- My li tm: c th t tc 3.200 vng/pht
- Thanh khuy: c bao bng Teflon, kch thc 1 inch
- My khuy t
Ho cht, thuc th:
- Toluen tinh khit
- Natri Vitride TM [ natri bis (2-methoxyethoxy) nhm
dihydrid, thng xp x 70% trong toluen (khong 3,5
mol/l)] (Tp on ho cht Fluka ., Hauppage, NY, M). Ly
10 ml cho vo bnh nh mc dung tch 100 ml. Pha n
42
QCVN 4-22: 2011/BYT

th tch 100 ml bng toluen v lc u.
- Dung dch thu phn: Thm t t 50 ml dung dch H 2SO4
m c, tinh khit vo 200 ml nc ct ng thi khuy
trong chu nc . Lm ngui ti nhit phng.
- Dung dch phenolphthalein: 1% trong ethanol.
- Dung dch NaOH: Ho tan 16 g NaOH trong 70 80 ml
nc ct v lm ngui ti nhit phng. Pha ti 100 ml
bng nc ct v lc u. trong bnh polyethylen.
- 1, 4- Butandiol: 99%
- Glycerol: 99%
- Dung dch ni chun: Cn 0,1 g 1, 4- butandiol cho vo
bnh nh mc dung tch 100 ml. Pha ti th tch 100 ml
bng nc ct v lc u.
- Dung dch glycerol: Cn 0,1 g 1, 4- butandiol v 0,1 g
glycerol cho vo bnh nh mc dung tch 100 ml. Pha ti
th tch 100 ml bng nc ct v lc u.
iu kin chy sc k kh:
I (alcol nha)
Nhit :
- Ct: 1900C, ng nhit
- u vo: 2500C
- Detector: 2500C
Tc dng:
- Kh mang (He): 30 ml/pht ti 63 psi
- H2: 30 ml/pht
- Khng kh: 240 ml/pht
II (glycerol)
Nhit :
- Ct: t theo chng trnh, 120 200 0C vi tc
60C/pht
- u vo: 2500C
- Detector: 2500C
Tc dng:
- Kh mang (He): 30 ml/pht ti 63 psi
- H2: 30 ml/pht
- Khng kh: 240 ml/pht
Cch tin hnh I (i vi nha):
Cn 250 300 mg mu cho vo bnh tam gic dung tch 25
ml c thanh khuy t. Dng pipet ly 5,0 ml toluen cho vo
bnh v khuy t cho n khi mu c ho tan. Ly 5,0
ml Natri VitrideTM cho vo bnh, y np bnh v khuy
trong 30 pht. M np ra ng thi khuy, dng pipet ly
3,0 ml dung dch thu phn cho vo bnh. Tip tc khuy
trong 3 pht. Chuyn hn hp trong bnh vo ng li tm,
43
QCVN 4-22: 2011/BYT

y np v lc u. Cho thot kh v li tm vi tc 2.800
3.200 vng/pht trong 5 pht. Bm 0,5 l lp trn vo
thit b sc k kh vi cc iu kin k thut t v ghi
sc k . So snh vi cc sc k c biu th pha
di xc nhn th t thi gian lu ca cc alcol nha.
Cch tin hnh II (i vi glycerol)
Dung pipet hoc syringe hypodermic, loi b lp toluen v
mt phn dung dch nc v li khong 2 ml dung dch
nc trong ng li tm. Thm 1 git dung dch
phenolphthalein v trung ho bng dung dch NaOH. Cc
mui nhm s kt ta. Dng pipet ly 5 ml dung dch ni
chun cho vo ng, pha n 15 ml bng nc ct, y
np, lc v li tm vi tc 2.800 3.200 vng/pht trong
5 pht. Bm 1 l dch trong trn b mt vo thit b sc k
kh vi cc iu kin k thut t v ghi sc k . Bm
1 l dung dch glycerol v ghi sc k . o cc thi gian
lu ca bt k cc pic so vi 1,4- butandiol. So snh cc
thi gian lu vi thi gian lu ca glycerol.
6.2. tinh khit
Khng c nha du cao
(Lu hunh)
Khi cc hp cht hu c c cha lu hunh c gia nhit

vi s c mt ca natri format, lu hunh chuyn ho
thnh hydrogen sulfid c pht hin bng cch s dng
giy ch acetat. Php th dng tnh cho thy vic s
dng nha du cao thay cho nha g.
Thit b, dng c:
- ng th: loi tiu chun, kch thc 10 x 70 mm, lm
bng thu tinh chu nhit.
- n Bunsen: Thng dng c nh dng ngn la nh
Ho cht, thuc th:
- Dung dch natri format: Ho tan 20 g natri format tinh khit
(NaOOCH) trong 100 ml nc ct.
- Giy th ch acetat: dng thng mi c sn ca hu ht
cc nh cung cp ho cht
Cch tin hnh:
Cn 40 50 mg mu cho vo ng th v thm 1 -2 git
dung dch natri format 20% (khi lng/th tch). di
giy th ch acetat trn ming ng th. Gia nhit ng th
bng ngn la cho n khi khi c hnh thnh v tip
xc vi giy th. Tip tc gia nhit trong 2 5 pht. Khng
c c m en ca ch sulfid hnh thnh, nu c m
en th chng t s c mt ca cc hp cht cha lu
hunh. (Gii hn pht hin: 50 mg/kg lu hunh).
44
QCVN 4-22: 2011/BYT

im nng chy
im nng chy c nh ngha l nhit ti mt a

mu c gi bn trong mt chic nhn nm ngang gim
xung mt khong 25,4 mm di trng lng ca mt cu
thp khi mu c gia nhit vi tc qui nh trong chu
cch thy hoc cch glycerol.
Thit b:
Thit b c minh ho trong Hnh 1 v Hnh 2 gm c cc
b phn c m t trong cc phn di y.
Chic nhn: c lm bng ng thau ph hp vi kch
thc trnh by trong Hnh 1a. Nu cn, vng c th c
gn bng cch hn hoc cch khc thun tin vi mt dy
ng thau loi 13 B&S (ng knh 0,06 0,08 inch hoc
1,52 2,03 mm) c trnh by Hnh 2a.
Qu cu: thng dng qu cu c lm bng thp c
ng knh 3/8 inch (9,53 mm), khi lng 3,45 3,55 g.
Hng dn chnh tm qu cu: Hng dn chnh tm qu
cu c lm ng thau v c hnh dng, kch thc
chung c minh ha trong Hnh 1c, c th c s dng
nu mun.
Dng c cha:
S dng bnh thu tinh chu nhit nh cc Griffin dng ln
dung tch 800 ml, ng knh khng c nh hn 3,34
inch (8,5 cm) v chiu su tnh t y n phn loe ra
khng c nh hn 5 inch (12,7 cm).
Dng c gi chic nhn v nhit k:
Bt k dng c hu hiu no ph hp vi cc yu cu sau
dng gi vng v nhit k u c th c s dng: (1)
Vng nhn c th c gi v tr nm ngang; (2) khi s
dng thit b m t trong Hnh 1d, y ca vng trn nm
trn v cch tm nm ngang pha di 1 inch (25,4 mm),
b mt y ca tm nm ngang cch t nht 0,5 inch (13
mm) v khng c qu 0,75 inch (18 mm) so vi y ca
dng c cha bn trn, chiu su ca dch lng trong
dng c cha khng c nh hn 4,0 inch (10,2 cm); (3)
khi s dng thit b a ra Hnh 1e, y ca vng trn
cch 1 inch (25,4 mm) so vi y ca dng c cha pha
trn, vi im di cng ca thanh ngh t trn y ca
dng c cha v chiu su ca dch lng trong dng c
cha khng c nh hn 4,0 inch (10,2 cm) nh m t
Hnh 1 a, b v c; (4) trong c hai dng c, nhit k c
treo ln sao cho khong cch t y ca bu nhit k n
y ca chic nhn khong 0,5 inch (13 mm) nhng khng
c chm vo nhn.
Nhit k thu ngn:
Ph thuc vo im nng chy ca mu, s dng hoc
nhit k ASTM 15C (-2 n 800C) i vi loi c im
nng chy thp hoc nhit k ASTM 16C (30 - 200 0C) i
vi loi c im nng chy cao .
45
QCVN 4-22: 2011/BYT

My khuy:
S dng my khuy thch hp vi tc 500 700
vng/pht. m bo phn tn nhit u trong mi
trng nng, hng ca trc quay nn y dch lng ln
pha trn. (Xem Hnh 2d ).
Chun b mu:
Ly mu i din gm cc mnh va mi b v c b mt
cha b oxy ho. No lp trn b mt mu thu cc
mnh v ngay trc khi s dng, trnh bao gm cc bt
mn hoc bi. Lng mu ly thng t nht gp i lng
cn cho s chic nhn yu cu nhng khng c
nh hn 40 g. Ngay sau lm nng chy mu trong dng
c cha sch, s dng t sy, tm gia nhit hoc cch ct
hoc cch du ngn qu nhit cc b. Trnh hnh thnh
bt kh trong mu nng chy, khng c gia nhit trn
nhit cn thit mu d dng m khng bao gm
bt kh. Thi gian tnh t lc bt u gia nhit cho n lc
mu khng qu 15 pht. Ngay trc khi y cc
chic nhn, gia nhit mu trc n nhit ti mu
c rt. Trong khi rt, cc vng trn c gi trn tm
ng thau. Rt mu vo cc vng trn tha cho ngui.
Lm ngui t nht 30 pht v sau ct b phn mu tha
bng dao h nng hoc dao bay. S dng dng c
cha sch v mt mu mi nu php th c lp li.
Cch tin hnh:
Mu c im nng chy trn 800C: Rt glycerol vo bnh
thu tinh ti su khng c nh hn 4 inch (10,2 cm)
v khng c qu 4,25 inch (10,8 cm). Nhit ban u
ca chu l 320C. i vi nha thng (gm c nha g),
glycerol cn c lm ngui n nhit khng c nh
hn 450C di im nng chy d on trc nhng
khng c thp hn 350C. V tr trc ca trc khuy gn
thnh sau ca dng c cha, vi cc li dao khng chm
vo thnh v phn di ca cnh dao cch nh ca vng
0,75 in (18 mm). Tr khi c hng dn chnh tm cu
c s dng, lm lm nh trung tm ca mu bng
cch nhn qu cu hoc mt que trn c h nng
dng cho mu cng, vo mu ti thi im ny. Treo vng
trn c cha cc mu trong chu glycerol b mt di
ca vng trn y cch b mt ca tm ngang thp hn l
1,0 inch (25,4 mm) (xem Hnh 1d), t nht 0,5 inch (13 mm)
v khng qu 0,75 inch (18 mm) trn so vi y ca bnh
thu tinh, hoc 1,0 inch (25,4 mm) trn so vi y ca
dng c cha (xem Hnh 2e). t qu cu trong glycerol
nhng khng c t ln trn mu th. Treo nhit k
ASTM 16C trong glycerol sao cho y bu ca nhit k
cch y chic nhn khong 0,5 inch (13 mm) nhng
khng c chm vo chic nhn. Duy tr nhit ban u
ca glycerol trong 15 pht v sau dng kp thch hp
t qu cu vo trung tm b mt trn ca mu trong
chic nhn. Bt u khuy v tip tc khuy vi tc 500
46
QCVN 4-22: 2011/BYT

700 vng/pht cho n khi hon tt vic xc nh. Gia
nhit theo tc tng nhit ca glycerol 5 0C/pht, trnh
nh hng ca cn bng cch s dng cc tm chn nu
cn thit.
[Ch : Tc tng nhit s khng i v s khng c
tnh theo gi tr trung bnh trong ton b qu trnh th. Loi
b tt c cc php th trong tc tng nhit vt qu
0.5C cho bt k qu trnh no sau 3 pht u].
Ghi li im nng chy, chnh l nhit trn nhit k ti
mu chm vo tm nm ngang pha di (xem Hnh
1d) hoc y ca dng c cha (xem Hnh 2e). Khng hiu
chnh thn nhit k.
Mu c im nng chy di 80 0C: thc hin theo cch
tin hnh trn, ngoi tr s dng nhit k ASTM 15C v s
dng nc va un si c lm mt ti 5 0C to mi
trng nhit. i vi nha thng (gm c nha g), s
dng nc c lm ngui n nhit khng c nh
hn 450C di im nng chy d on trc nhng
khng c thp hn 50C.
Ch s hydroxyl
Ch s hydroxyl c nh ngha l s mg KOH dng

trung ho carbamat sulfonyl c kh nng kt hp vi cc
nhm hydroxyl trong 1 g mu. Cc nhm hydroxyl trong
hp cht hu c phn ng nhanh vi p toluensulfonyl
isocyanat d (p - TSI) trong dung mi tr to thnh
carbamat sulfonyl. Sau phn ng ca thuc th d vi
nc to thnh p toluensulfonamid, carbamat sulfonyl c
tnh acid c chun bng trc quan hoc thit b
chun bng dung dch KOH trong methanol, pht trin
im tng ng bng o th hoc bng ch th mu.
Cc hiu chnh c thc hin i vi mu trng v s c
mt ca bt k cc hp cht c tnh acid.
Thit b, dng c:
- Thit b chun t ng: s dng thang o pH 0 14,
t tc 4 (khong 2 ml/pht) v mt buret 20 ml.
- in cc thu tinh
- in cc calomel
- Bnh tam gic: dung tch 250 ml c khp ni thu tinh
hnh trn
- Sinh hn Allihn: di 300 mm c khp ni thu tinh hnh
trn khp vi bnh tam gic.
Ho cht, thuc th:
- Acid benzoic, t tiu chun cht chun gc
- Methanol, tinh khit, dng khan
- Toluen, tinh khit, sy kh qua ry phn t 3
- KOH 0,1 N pha trong methanol: Ho tan 7 g KOH trong 1
lt methanol.
Chun ho bng cch cn chnh xc n 0,0001 g, khong
47
QCVN 4-22: 2011/BYT

0,12 g acid benzoic vo cc dung tch 150 ml. Cho thanh
khuy t v 80 ml hn hp toluen/methanol theo t l 1/1.
Khuy u dung dch trong khi chun vi dung dch
KOH trong methanol. Dung dch KOH cn phi cho xung
di b mt ca dung dch, cch xa in cc. Tnh ton
nng dung dich KOH trong methanol da theo phng
trnh tnh ton c biu th di y.
- Tetrahydrofuran (THF): sy qua m v cho qua ry phn
t 3
- p-Toluenesulfonyl isocyanat (p-TSI)
- Dung dch p-Toluenesulfonyl isocyanat: khong 0,22 M
hoc 4,5 mEq/20 ml dung dch. Dng pipet ly 15 ml pToluenesulfonyl isocyanat (p-TSI)
cho vo 500 ml
tetrahydrofuran (THF) kh v lc u.
Ch :
V isocyanat c bn cht rt c nn khi chun b v s
dng dung dch isocyanat phi c tin hnh trong t ht.
Cn phi eo gng tay khi cm vo isocyanat v dung dch
ca isocyanat trnh tip xc vi da.
- Dung dch ch th bromocresol ta: cho 0,1 g
bromocresol ta vo 18,5 ml dung dch NaOH 0,1 N v
pha ti th tch 250 ml bng nc ct.
Cch tin hnh:
Cn 1 - 1,5 g mu chnh xc n 0,0001 g cho vo bnh
tam gic kh dung tch 250 ml c ni vi khp ni thu
tinh hnh trn. Dng pipet ly 10 ml dung dch THF kh cho
vo bnh v ho tan mu. Dng pipet ly 20 ml dung dch p
TSI cho vo bnh v lc u. Cho vi ht bt, ni vi
sinh hn v bnh trn tm gia nhit. Gia nhit n khi si
vi sinh hn ngc trong 10 pht. Trong qu trnh chng
ct b sung thm nc thch hp qua sinh hn:
Mu trng
Mu th
Chun vi ch th mu
2
2
Chun bng o th
1
1
Ly bnh v sinh hn ra khi tm gia nhit v ngui ti
nhit phng. Ra sinh hn bng 5 ml THF. Tho sinh
hn ra khi bnh v chuyn ton b phn dch trong bnh
vo cc dung tch 150 ml vi s tr gip ca 50 ml THF.
Cho thanh khuy t v nhng cc in cc vo hoc thm
20 git dung dch ch th. Va khuy va chun bng
thit b chun o th hoc chun vi ch th mu trc
quan vi dung dch KOH trong methanol. Dung dch KOH
48
QCVN 4-22: 2011/BYT

cn phi cho xung di b mt ca dung dch cch xa
in cc. Xc nh th tch dung dch KOH dng
chun mu th v chun mu trng c thc hin
qua tt c cc bc tin hnh trn.
Tnh kt qu:
Nng ca dung dch KOH trong methanol (N):
Trong :
W: Khi lng acid benzoic
122,1: ng lng ca acid benzoic
KOH: S ml dung dch KOH trong methanol dng chun
Ch s hydroxyl trong mu:
Trong :
A: S ml dung dch KOH dng chun mu th
B: S ml dung dch KOH dng chun mu trng
N: Nng dung dch KOH trong alcol
56,1: S mg KOH/mEq
AV: Ch s acid
Asen
Chun b dung dch mu nh sau: Cn chnh xc 1 g mu

v cho vo bnh Kjeldahl, t u mt ng ca bnh trong
qu bu bc hi c gn vi my ht nc, thm 5 ml
dung dch H2SO4 v 4 ml dung dch hydrogen peroxyd 30%
v ph mu trn ngn la nh. Tip tc thm 2 ml peroxyd
trong 2 ln, phn ng lng cn gia hai ln thm cho
n khi tt c cht hu c b ph hu, khi ca acid H 2SO4
bc ra mnh v dung dch tr ln khng mu. Duy tr cc
iu kin xy ho ti tt c cc thi im trong qu trnh
ph mu bng cch b sung peroxyd mi khi hn hp
chuyn mu nu hoc ti mu. (Lng peroxyd cn ph
hon ton mu s thay i nhng trong mt s trng hp
mc ti a c th l 200 ml, iu ny ph thuc vo trng
thi t nhin ca mu). Lm ngui, ch thm 10 ml nc,
li cho bc hi n khi to thnh khi mnh v lm ngui.
Chuyn dung dch ti bnh to arsin, ra bnh Kjeldahl v
qu bu bng nc, thm nc ra vo bnh v pha ti 35
ml bng nc. Dung dch ny phi p ng c cc yu
cu ca Gii hn th arsenic.
Ch
Cn chnh xc 5 g mu v cho vo a s hoc bt s, un

trn tm gia nhit cho n khi than ho hon ton, sau
gia nhit trong l nung 480 0C 8 gi hoc qua m,
ngui. Thm cn thn 5 ml acid nitric, lm bay hi n kh
49
QCVN 4-22: 2011/BYT

trn tm gia nhit, sau nung trong l nung 480 0C
trong 15 pht, v lm ngui. Trch ly tro trong 10 ml nc
trong 2 ln, lc mi phn dch chit vo mt bnh gn. Lc
qua bt k cht khng tan trn dng c lc bng 6 ml dung
dch amoni citrat TS, 2 ml hydroxylamin hydrochlorid TS v
5 ml nc, thm nc ra c lc vo bnh gn. Tip
tc theo hng dn trong phn Cch tin hnh trong th
Gii hn, bt u vi Thm 2 git phenol TS .... vo
bnh gn, s dng 10 g ion ch (Pb) trong mu i
chng.
Ph hng ngoi
Glycerol ca nha g thng
Sc k kh ca cc alcol
nha thng
50
QCVN 4-22: 2011/BYT
Thit b, dng c - im
nng chy
Hnh 1
Hnh 2
51
QCVN 4-22: 2011/BYT

Ph lc 12
I VI DINATRI DIPHOSPHAT
1. Tn khc, ch s
Disodium pyrophosphate; Disodium dihydrogen

diphosphate; acid sodium pyrophosphate.
INS 450i
MTDI=70mg/kg th trng tnh cho Phospho t cc ngun
thc phm
2. nh ngha
Tn ha hc
Disodium dihydrogen diphosphate; Disodium dihydrogen

pyrophosphate
Ch s C.A.S.
7758-16-9
Cng thc ha hc
Dng khan: Na2H2P2O7
Khi lng phn t
221,94
3. Cm quan
Dng tinh th hoc ht mu trng.
4. Chc nng
Cht nh ha, m, cht to phc kim loi, cht to xp
5. Yu cu k thut
5.1. nh tnh
tan
Tan trong nc.
pH
3,7-5,0 (dung dch 1/100).
Natri
Phi c phn ng c trng ca natri.
Phosphat
5.2. tinh khit

Gim khi lng khi sy
kh
Khng c qu 0,5% (105oC trong 4 gi)

nc
Khng c qu 1%.
Fluorid
Khng c qu 10,0 mg/kg
Arsen
Khng c qu 3,0 mg/kg
Ch
Khng c qu 4,0 mg/kg
5.3. Hm lng
Na2H2P2O7
Dng khan, hemihydrat v monohydrat: khng thp hn

97,0% tnh theo ch phm khan.
Dng dodecahydrat: khng thp hn 92,0% tnh theo ch
phm sau khi nung.
6. Phng php th
52
QCVN 4-22: 2011/BYT

6.1. tinh khit
nc
Ha tan 10 g mu th trong 100 ml nc nng. Lc qua

mt chn lc cn b. Ra cn khng tan trn chn lc
bng nc nng. Sy kh ti (105oC trong 2 gi). ngui
v cn.
6.2. nh lng
Cn 400mg (chnh xc n mg) mu th c sy kh

trc ti (105oC trong 4 gi), ha tan trong 100 ml nc
trong cc 400 ml. Chnh pH dung dch v 3,8 bng dung
dch acid hydrocloric long (TS) hoc dung dch natri
hydroxyd (TS), dng pH k xc nh pH dung dch. Sau
thm 50 ml dung dch km sulfat (125 g ZnSO 4.7H2O
ha tan trong nc, pha long n 1000ml, lc v chnh
pH v 3,8), yn trong khong 2 pht. Chun acid
c gii phng bng dung dch natri hydroxyd 0,1 N n
khi pH dung dch li tr v 3,8. Sau mi ln thm natri
hydroxyd gn n im tng ng, cn mt thi gian
nu c kt ta km hydroxyd th kt ta c th tan ht.
Mi ml natri hydroxyd 0,1 N tng ng vi 11,10mg
Na2H2P2O7.
53
QCVN 4-22: 2011/BYT

Ph lc 13
I VI CALCI POLYPHOSPHAT
1. Tn khc, ch s
2. nh ngha
INS 452iv
MTDI=70mg/kg th trng tnh cho phospho t cc ngun
thc phm
Hn hp d th ca cc mui calci ca acid polyphosphoric
c cng thc chung l Hn+2PnOn+1.
3. Cm quan
Tinh th hoc bt khng mi, khng mu.
4. Chc nng
Cht nh ha, Cht gi m, cht to phc kim loi, cht to

kt cu.
5. Yu cu k thut
5.1. nh tnh
tan
Thng khng tan hon ton trong nc, tan trong mi

trng acid.
Phosphat
Calci
Phi c phn ng c trng ca calci (Dch th chun b

nh trong phn th phosphat)
5.2. tinh khit

o
Gim khi lng khi nung Khng c qu 2%. Sy ti 105 trong 4 g sau nung
ti 550o trong 30 pht.
Phosphat vng
Khng c qu 8% tnh theo hm lng P2O5.
Fluorid
Arsen
Ch
5.3. Hm lng P2O5
Khng c thp hn 50,0% v khng c qu 71,0%

P2O5 tnh theo ch phm sau khi nung.
6. Phng php th
6.1. nh tnh
Phosphat
Cn 0,5g mu, trn vi 10ml acid nitric v 50ml nc. un

si trong 30 pht v lm mt. Dung dch ny c s dng
lm dch th.
6.2. tinh khit

Arsen
- Th theo hng dn ti JECFA monograph 1 - Vol.4 phng php II,.

- Ha tan 1 g mu th trong 15 ml dung dch acid
hydrocloric long (TS), thm 20 ml nc, dung dch ny
c s dng lm dch th).
54
QCVN 4-22: 2011/BYT

Ch

6.3. nh lng
Cn khong 300 mg mu th, chnh xc n mg, ha tan

trong 15 ml acid nitric v 30 ml nc ct. un si trong
khong 30 pht, pha long vi nc n 100 ml. un nng
n 60oC, thm lng d dung dch amoni molybdat (TS)
v un 50oC trong 30 pht. Lc v ra kt ta bng acid
nitric long (dung dch 1/36), tip theo bng dung dch kali
nitrat (1/100) n khi dch ra khng cn acid vi qu tm.
Ha tan kt ta trong 50 ml dung dch natri hydroxyd 1N,
thm dung dch phenolphtalein (TS) v chun lng
natri hydroxyd d bng acid sulfuric 1N.
Mi ml dung dch natri hydroxyd 1 N tng ng vi
3,086mg P2O5.
55
QCVN 4-22: 2011/BYT

Ph lc 14
I VI CC MUI CA CC ACID BO
1. Tn khc, ch s
Salts of fatty acids

INS 470
ADI khng gii hn
2. nh ngha
Cc sn phm ny cha mui calci, kali v natri ca cc acid

myristic, oleic, palmitic, stearic hoc hn hp cc acid ny
thu c t m v du n. Sn phm thng mi cn c
phn loi da trn:
- Ch s x phng ha;
- im ng c ca cc acid bo thu c t mu th;
- Ch s iod;
- Cn cn li sau khi nung bao gm c hm lng cc
cation;
- m.
3. Cm quan
Tinh th rn hoc na rn, bng, mu trng hoc vng nht,

hoc bt mu trng hoc trng vng.
4. Chc nng
Cht chng ng vn, Cht nh ha.
5. Yu cu k thut
5.1. nh tnh
tan
Cc mui kali v natri tan trong nc v ethanol, cc mui

calci khng tan trong nc, ethanol v ether.
Cation
Phi c phn ng c trng ca cation.
Thnh phn acid bo
Phi c phn ng c trng ca thnh phn acid bo
5.2. tinh khit

Cc acid bo t do
Khng c qu 3%
Cc cht khng x
phng ha
Khng c qu 2 %.
Ch
5.3. Hm lng
Khng thp hn 95 % tng cc mui acid bo, tnh theo khi

lng kh.
6. Phng php th
6.1. nh tnh
Cation
un nng 1 g mu th vi hn hp gm 25 ml nc v 5 ml
acid hydrocloric. Cc acid bo to thnh lp ni trn b mt
thnh mt lp rn hoc du, tan trong hexan. Sau khi lm
56
QCVN 4-22: 2011/BYT

ngui, gn ly lp nc v cho bay hi n kh. Ha tan
cht rn cn li trong nc v th cc cation thch hp.
57
QCVN 4-22: 2011/BYT

Thnh phn acid bo
S dng phng php nh lng nh tnh ring cc acid

bo c trong thnh phn ca mu. Cc acid bo chim lng
ln nht phi ph hp vi cc acid c a ra trn nhn
sn phm.
6.2. tinh khit

Cc acid bo t do
Xc nh cc acid bo t do theo hng dn trong phn

Phng php xc nh Acid bo t do. Tnh hm lng acid
bo t do, s dng h s tng ng (e) tng ng vi
1/10 khi lng phn t ca mui.
Cc cht khng x
phng ha
Cc cht khng x phng ha l ton b lng sn phm c

mt trong cc cht bo sau khi c x phng ha vi cc
hydroxyd kim loi kim v chit bng mt dung mi nht
nh, vn khng bay hi trong cc iu kin xc nh ca
php th.
Cc cht ny bao gm cc lipid c ngun gc t nhin nh
cc sterol, cc ru no mch di hn, cc phm mu v cc
hydrocarbon cng nh bt k mt tp cht khng bay hi
no 1030C c mt trong sn phm.
Cn khong 5 g mu th (chnh xc n 0,01g) c
trn u vo bnh cu y trn 250 ml. Thm 50 ml dung dch
kali hydroxyd ~ 0,5 N v thm mt t bt. Gn bnh vo
sinh hn hi lu, un si nh trong 1 gi. Ngng un. Thm
100 ml nc ct qua u sinh hn v lc.
Sau khi lm mt, chuyn dung dch vo phu tch. Trng ra
bnh v bt vi ln bng diethyl ether (dng khong 100
ml) v dch ra vo phu tch. ng nt v lc mnh
trong 1 pht, u n x p sut bng cch lt ngc phu
tch v m kha vi.
yn phu tch cho n khi 2 pha han ton tch lp. Sau
rt ly cng trit cng tt dung dch x phng vo phu
tch th 2.
Chit dung dch x phng trong ethanol thm hai ln na,
mi ln vi 100 ml diethyl ether theo cch trn. Gp 3 dch
chit ether vo 1 phu tch c sn 40 ml nc.
Nh nhng quay trn phu tch cha dch chit v 40 ml
nc. Nu lc qu mnh trong giai on ny, nh tng c
th hnh thnh. hn hp tch lp hon ton v rt b lp
nc di. Ra lp ether hai ln na vi 40 ml nc, lc
u v loi b lp nc di sau khi hn hp phn lp.
Vi mi dung dch ra rt ra n khi ch cn khong 2 ml,
sau quay trn phu tch quanh trc, i vi pht, rt b
phn tch ra, ng kha vi khi ether bt u chy qua l
ca kha vi.
Ra dung dch ether nhiu ln bng 40 ml dung dch kali
hydroxyd, 40 ml nc, ra thm mt ln bng 40 ml dung
dch kali hydroxyd, sau ra t nht 2 ln na bng 40 ml
nc. Lin tc ra bng nc cho n khi dung dch ht
mu hng khi th bng ch th l dung dch phenophthalein.
58
QCVN 4-22: 2011/BYT

Chuyn ton lng tng t mt dung dch ether qua cung
ca phu tch vo bnh cu kh v cn b khi lng
chnh xc n 0,0001 g.
Lm bay hi dung mi bng cch ct trong b cch thy.
Thm 5 ml aceton v loi b hon ton dung mi bay hi
bng cch thi khng kh nh, nghing bnh cu khi quay
trong b cch thy.
Sy kh phn cn cn li nhit 1032C trong 15 pht,
t bnh cu theo phng gn nh nm ngang. Lm ngui
trong bnh ht m v cn (chnh xc n 0,0001 g). Lp li
qu trnh sy trong mi 15 pht lin tip cho n khi chnh
lch gia 2 ln cn lin tip nh hn 0,0015g.
Ch : Nu khng thu c khi lng khng i sau 3 ln
sy kh, cc cht khng x phng ha c th b nhim
bn.
Sau khi cn, ha tan phn cn trong 4 ml diethyl ether,
thm 20 ml ethanol c trung ha (dung dch c mu
hng khi thm ch th l dung dch phenolphthalein(TS).
Chun bng dung dch kali hydroxyd trong ethanol 0,1 N
chun ha (pha dung dch kali hydroxyd trong ethanol c
nng gn ng 1 N bng cch ha tan 60 g kali hydroxyd
trong 50 ml nc v pha long thnh 1 L bng ethanol; pha
long dung dch ny 1:10 bng ethanol) n khi dung dch c
mu pht hng.
Hiu chun khi lng cn cn li bng cch tr i hm
lng acid t do. Tnh hm lng cht khng x phng ha,
theo % (kl/kl) bng cng thc sau:
trong :
m = khi lng (g), ca phn mu th,
m1 = khi lng (g), ca cn cn li.
V = th tch dung dch kali hydroxyd chun ha nng
dng chun .
T = Nng chnh xc ca dung dch kali hydroxyd dng
chun .
59
QCVN 4-22: 2011/BYT

Ch

6.2. nh lng
Nguyn tc:
X phng ha cc mui v ester ha cc acid bo bng
methanol, c mt bo trifluorid, methanol kim. Tin hnh sc
k lng kh cc ester methyl ca acid bo.
Phn A - Chun b cc ester methyl ca acid bo
Thit b
- Bnh y trn c nhm 50 v 100 ml.
- Sinh hn hi lu, chiu di hiu dng 20 to 30 cm, c khp
ni nhm tng thch vi bnh cu.
- Cc phu tch 250 ml.
- ng ng vo dn kh nitrogen.
- ng nghim c nt thy tinh nhm.
- Pipet chia , c th tch t nht l 10 ml, c gn qu bp
cao su, hoc pipet t ng.
Thuc th
- Heptan, dng cho sc k (Ch 2 v 4)
- Du nh c ct li (nhit si t 40-60), ch s
brom < 1, khng c cn, hoc hexan (Ch 2)
- Natri sulfat khan
- Dung dch Natri hydroxyd trong methanol ~ 0.5 N: Ha tan
2g natri hydroxyd trong 100 ml methanol cha khng qu
0.5% (kl/kl) nc. Nu gi dung dch tng i lu c th to
thnh mt lng nh kt ta mu trng ca natri. iu ny
khng nh hng n kt qu iu ch methyl ester.
- Dung dch bo trifluorid trong methanol, 12 n 25% (kl/kl) .
Ch phm thng mi sn c l dung dch 14 v 50% (ch
2)
Cnh bo: Bo trifluorid c. V vy th nghim vin khng
nn pha dung dch bo trifluorid trong methanol t methanol
v boron trifluorid. (ch 3).
- Dung dch bo ha natri clorid trong nc.
- Methyl , dung dch 1 g/l trong ethanol 60% (tt/tt)
- Nitrogen, c hm lng oxy < 5 mg/kg
Tin hnh
Do bo trifluorid c, cc th nghim sau tt nht nn tin
hnh trong t ht. Cc dng c thy tinh phi c ra bng
nc ngay sau khi s dng.
Sy kh mu nhit 105C n khi lng khng i, c
60
QCVN 4-22: 2011/BYT

2 gi th kim tra khi lng 1 ln. Cn khang 350mg
(chnh xc n mg) mu sy kh. C th ly lng mu
ln hoc nh hn 350 mg, tuy nhin, th tch ca bnh cu v
lng thuc th s dng phi ph hp vi s liu trong bng
sau:
Khi lng
NaOH 0.5 Dung dch BF3
Th tch bnh
mu
N
trong methanol
(mg)
(ml)
(ml)
(ml)
100-250
50
4
5
250-500
50
6
7
500-700
100
8
9
750-1000
100
10
12
Cho lng acid bo nh vo bnh cu ph hp. Thm
vi lng ph hp dung dch bo trifluorid trong methanol.
un si trong vng 2 pht.
Thm 2 n 5 ml heptan (ch 4) (lng chnh xc khng
nh hng n phn ng) qua u trn ca sinh hn vo
hn hp ang si v tip tc un si trong 1 pht.
Ngt ngun nhit, ly sinh hn ra. Thm lng nh dung dch
natri clorid bo ha v lc nh bnh bng cch quay trn bnh
vi ln.
Thm dung dch natri clorid bo ha vo bnh cu sao cho
mc cht lng ngang c bnh. yn cho hn hp tch lp
v chuyn khong 1 ml lp trn (lp heptan) vo ng nghim
c nhm v thm vo mt lng nh natri sulfat khan loi
ht nc. Nu lng mu ly l 350 mg, dung dch ny cha
khong 7-17% methyl ester v c th bm trc tip vo ct
sc k kh-lng. Nu khng th pha long dung dch bng
heptan t c nng methyl ester l 5-10% (ch 5).
thu hi ton b lng ester kh, chuyn dung dch mui
v lp heptan vo phu tch. Tch ring cc lp. Chit phn
dung dch mui 2 ln bng 50 ml du nh. Gp dch chit du
nh thu c vo phn dung dch heptan, ra bng 20 ml
nc n khi ht acid (th bng ch th methyl). Lm kh
bng natri sulfat khan, lc v cho bay hi dung mi trong b
cch thy v thi kh nitrogen (ch 6 v 7). Vi cc mu c
khi lng nh hn 500 mg phi gim th tch dung mi v
nc s dng theo t l tng ng.
Bn cnh phng php trn cn c mt s phng php
khc khng s dng n bo trifluorid. Nhn chung c th thay
cc thuc th methyl ha, dung dch natri hydroxyd 0,5N
trong methanol v dung dch bo trifluorid 12-25 %, trong
methanol bng cc cht sau:
- Kali hydroxyd 1 N trong methanol, (phn ng vi cht bo
khi c mt lng d methanol c hm lng nc nh);
- Dung dch natri methylat (iu ch bng cch ha tan 1 g
natri kim loi trong 100 ml methanol c hm lng nc
nh).
Ch
61
QCVN 4-22: 2011/BYT

1. Nu cc cht khng x phng ha gy cn tr, pha long
dung dch x phng ha vi nc v loi b cc cht khng
x phng ha bng cch chit vi diethyl ether hoc hexan.
Acid ha dung dch nc x phng v tch ly cc acid bo.
iu ch cc methyl ester t cc acid bo theo hng dn.
2. Khi o sc k kh lng ca cc methyl ester, mt s thuc
th, c bit l bo trifluorid trong methanol c th to nn
cc peak ngu nhin trn sc (trong vng cc ester c
mch C20-C22 nu dng bo trifluorid trong methanol). Do vy
cn phi kim tra li mi t thuc th mi bng cch iu
ch cc methyl ester ca acid oleic tinh khit, v o sc k.
Nu xut hin peak ngu nhin, phi b khng dng thuc
th. Cc thuc th khc nhau khng c php cho peak
gy nhiu n cc peak ca cc methyl ester ca cc acid
bo trong qu trnh chy sc k.
Dung dch bo trifluorid trong methanol phi c bo qun
trong t lnh.
3. Nu bt buc phi iu ch dung dch bo trifluorid t bo
trifluorid kh, nn dng phng php sau: Cn khi lng
ca bnh cu 2 L cha 1 L methanol. Lm lnh trong b .
Vn gi nguyn bnh trong b , sc kh BF 3 t chai kh
(cylinder) qua ng dn thy tinh vo dung dch methanol cho
n khi hp th c 125 g BF 3. Tin hnh th nghim trong
t ht. Phi cho BF3 chy qua ng thy tinh trc khi t
ng vo v rt ng ra khi methanol trnh trng hp
cht lng b ht vo h thng van ca chai kh. Khng c
cho kh chy nhanh qu c hi kh trng ra khi bnh.
Thuc th pha theo cch ny bn trong 2 nm.
4. Nu cc acid bo cha 20 hoc nhiu hn 20 nguyn t
carbon khng c mt, nn thay heptan bng hexan (hn hp
ca cc ng phn C7 tinh khit c th c kim tra bng
sc k kh lng)
5. Nu khng c lng mu nh yu cu, c th ly 10
mg, thm ch t hn, min l lng thuc th v kch c ca
cc dng c thy tinh c gim theo t l tng ng.
6. Cc dung dch methyl ester nn c phn tch cng sm
cng tt. Nu cn, bo qun dung dch heptan cha cc
methyl ester trong mi trng kh tr trong t lnh. Nu cn
phi bo qun trong thi gian di, nn bo v cc methyl
ester khi s oxy ha bng cch thm vo dung dch cc
cht chng oxy ha nng khng nh hng n kt qu
phn tch, v d nh 0,05 g/L EHT (2,6-di-tertbutyl-4-methyl
phenol).
Trong trng hp cn thit, c th bo qun cc methyl ester
kh sch dung mi trong kh tr trong t lnh trong 24 gi,
hoc c th bo qun lu hn nu gi ng lnh su trong
ng kn trong chn khng.
7. Mt phn cc methyl ester d bay hi nht c th b mt
nu thi gian bay hi dung mi ko di, hoc nu dng kh
nitrogen qu mnh,
62
QCVN 4-22: 2011/BYT

o ph hng ngoi, phi loi b dung mi cng trit
cng tt.
o sc k kh lng, loi b hon ton dung mi.
Phn B - Sc k kh lng ca cc ester methyl acid bo
Thit b
Thit b thng thng dng cho sc k kh lng, dng ct nhi
v detector ion ha ngn la (ch 1). Bt k mt thit b
no cho hiu qu v phn gii cao vi cht bo cn xc
nh u ph hp.
Sc k kh lng
H thng bm mu: H thng bm mu phi c khng gian
cht nh nht c th. Nu c, phi nng c nhit
cao hn nhit ct t 20 n 50C.
L: L phi cung cp cho ct nhit t nht l 220 o v phi
duy tr c nhit cn thit trong khong 1C.
Nu dng chng trnh t nhit , nn dng thit b c ct
i.
Ct nhi:
- Ct: Ct phi c lm t lai vt liu tr vi cht cn phn
tch: thy tinh hoc nu khng th dng thp khng r (ch
2). Chiu di: 1 n 3 m, nn dng ct tng i ngn nu
c cc acid mach di (C20+). xc nh cc acid bo C4 v
C6, nn dng ct 2 m; ng knh trong t 2 n 4 mm.
Nhi ct
- Cht mang: Diatomid ra acid v c silan ha, hoc
cc cht mang tr ph hp khc c khong bin thin
ng knh hp (25m) trong khong ng knh c ht t
125-200 m, c ht trung bnh phi tng quan vi ng
knh trong v chiu di ct.
- Pha tnh: Dng polyester ca mt cht lng phn cc (v d
diethylen glycol polysuccinat, butandiol polysuccinat, ethylen
glycol polyadipat ...) hoc bt k cht lng no khc (v d
cyanosilicon ...) tha mn cc iu kin di y. Pha tnh
phi chim 5 n 20 % khi lng nhi. C th dng mt pha
tnh khng phn cc, ty theo tng php tch c th.
- Luyn ct mi ch to: Tch ct ra khi detector. Nu c
th, t t nung l n 185C v dn dng kh tr qua ct vi
tc 20-60 ml/pht trong t nht l 16 gi ti nhit ny,
v thm 2 gi na ti 195C.
Detector: Cc vn hnh di y tng ng vi detector ion
ha ngn la (ch 1)
Syring: Syring, c dung tch ti a l 10 l, chia n 0.1 l.
My ghi:
Nu s dng ng ghi tnh thnh phn hn hp phn
tch, phi dng mt my ghi in t c chnh xc cao.
63
QCVN 4-22: 2011/BYT

My ghi phi tng thch vi thit b o. Cc c trng ca
my ghi phi nh sau:
- Tc p ng di 1,5 giy, tt nht l di 1 giy (tc
p ng l thi gian cn bt ghi chy t 0 n 90 %
theo 100 % tn hiu)
- rng ca giy: ti thiu l 25 cm
- Tc giy: 25-100 cm/gi.
B tch phn Integrator hoc my tnh (ty chn)
C th tnh mt cch nhanh v chnh xc nu dng b tch
phn in t hoc my tnh. Trong trng hp ny phi to
c tn hiu tuyn tnh vi nhy ph hp, v phn hiu
chnh cho s lch ng nn phi tha ng.
Ha cht
- Kh mang: Kh tr (nitrogen, heli, argon ...) kh, v cha t
hn 10 mg/kg oxy.
- Kh ph tr: Hydrogen (tinh khit ti thiu 99.9%) khng c
cc tp cht hu c, khng kh hoc oxygen.
- Cc cht chun so snh: Hn hp ca cc methyl ester,
hoc cc methyl ester ca mt cht du bit trc thnh
phn, tt nht l tng t vi cht bo cn phn tch.
Tin hnh
iu kin th
Xc nh cc iu kin vn hnh ti u: Cc gi tr cho trong
bng 1 v 2 cho di y v nguyn tc c th cho cc kt
qu mong mun:
Bng 1
ng knh trong ca ct
Kh mang cung cp
2 mm
15-25 ml/pht
3 mm
20-40 ml/ pht
4 mm
40-60 ml/ pht
Bng 2
Nng ca pha tnh
Nhit
5%
175o
10%
180 o
15%
180 o
20%
185 o
Nu c, injector phi nhit khong 200 oC v detector
phi nhit bng hoc cao hn nhit ct.
V nguyn tc dng kh hydrogen cung cp cho detector ion
ha ngn la phi c tc bng mt na tc kh mang,
v tc kh oxygen phi bng khong 5 n 10 ln tc
kh hydrogen.
Xc nh hiu sut v phn gii (ty chn)
Tin hnh phn tch mu chun methyl stearat. La chn c
mu, nhit ct tch v tc kh mang sao cho peak ca
methyl stearat xut hin 15 pht sau peak dung mi v cao
khong 3/4 tn hiu ton thang.
64
QCVN 4-22: 2011/BYT

- Phn tch:
Dng mu kim tra l 0,1 n 2 l dung dch heptan ca
methyl esters, pha theo hng dn trong phn A. Trong
trng hp khng c cc ester trong dung dch, chun b
dung dch c nng khong 10% trong heptan v bm 0,1
n 1 l dung dch ny.
Cc iu kin tin hnh c cho di y. Tuy nhin, c
th lm vic vi nhit ct thp hn nu xc nh cc acid
c mch carbon di C12 hoc nhit cao hn nu xc
nh cc acid bo trn C20.
i khi c th s dng chng trnh t nhit cho c 2
trng hp trn. Nu mu c cha cc methyl ester ca cc
acid bo di C12, phi bm mu nhit 100C (hoc
nhit t 50 - 60C nu c acid butyric) v ngay lp tc
tng nhit vi tc tng nhit t 4 - 8 C/pht cho n
nhit ti u. Trong mt s trng hp c th gp c 2 qui
trnh li: sau khi tng nhit, tip tc ra gii ti nhit khng
i cho n khi tt c cc hp phn c ra gii ra. Nu
thit b khng vn hnh vi chng trnh nhit , lm vic
ti 2 nhit c nh trong khong t 100 n 195C.
Biu th kt qu
Phn tch nh tnh
Phn tch hn hp cht chun so snh c thnh phn
bit trong cc iu kin s dng o mu th. o khong
cch lu (hoc thi gian lu) cho cc ester bo tng ng.
Dng giy bn logarit, v th biu din s ph thuc ca
logarit khong cch lu (hoc thi gian lu) vo s nguyn
t carbon ca cc acid; trong iu kin ng nhit th ca
cc ester mch thng c cng khng bo ha (no) phi l
cc ng thng. gn nh song song vi nhau.
Nhn dng cc peak ca mu th t cc th ny, nu cn
th dng php ni suy. Phi trnh cc iu kin o lm xut
hin cc peak b che ph (masked peaks), c ngha l
phn gii khng ln tch c 2 hp phn.
Phn tch nh lng
Xc nh thnh phn
Tr cc trng hp c bit, s dng phng php chun
ha din tch, c ngha l gi thit rng ton b cc hp phn
u c biu din trn sc , sao cho tng din tch cc
peak biu din 100 % cc hp phn (tng ra gii).
Bng mt qui trnh chun ha ph hp (dng hn hp chun
so snh hoc dng cht chun ni), xc nh tng khi lng
ca cc acid bo trong mu kh. Tnh hm lng mui ca
cc acid bo vi cc cation c trng trong mu. Tng hm
lng Mui Acid Bo khng c ln hn 95% khi lng
mu kh. Ngoi ra, nu c cc ch tiu cho hm lng ca
mi acid bo ghi trn nhn sn phm, mu phi tha mn
c cc ch tiu ny.
Ch
65
QCVN 4-22: 2011/BYT

1. C th s dng my sc k kh - lng dng thit b o
dn nhit ca kh (catharometer) (lm vic trn nguyn tc
o s thay i dn nhit). Cc iu kin o khi c
thay i nh sau:
Ct
- chiu di: 2 n 4 m
- ng knh trong: 4 mm
- cht mang: ng knh ht trong khong 160 n 200 m
- pha tnh: 15 n 25%
Kh mang: heli, nu khng th dng hydrogen, c hm lng
oxygen cng nh cng tt. Khng dng kh ph tr
- Tc kh: thng trong khong t 60 n 80 ml/pht
Nhit
Injector: cao hn t 40o n 60oC so vi nhit ct
Ct: 180o to 200oC
Phn tch nh lng: phi hiu chnh theo cc h s thu
c khi phn tch hn hp so snh ca cc ester c thnh
phn bit trong cng iu kin o vi mu th.
2. Nu trong mu c cc thnh phn cha nhiu hn 3 ni
i, chng c th b phn hy trn ct thp khng r.
66
QCVN 4-22: 2011/BYT

Ph lc 15
I VI ESTER CA SUCROSE VI CC ACID BO
1. Tn khc, ch s
2. nh ngha
Sucrose fatty acid esters;

INS 473
Mono, di, tri ester ca sucrose vi cc acid bo thc
phm, c iu ch t sucrose v methyl, ethyl ester ca
cc acid bo thc phm bng cch ester ho vi s c
mt ca cht xc tc, hoc tch t sucroglycerid. Ch cc
dung mi sau c th c s dng sn xut:
dimethylformamid, dimethyl sulfoxid, ethyl acetat,
isopropanol, propylen glycol, isobutanol v methyl ethyl
keton.
3. Cm quan
Dng gel cng, dng cht c mm hoc dng bt c mu

trng n trng hi xm
4. Chc nng
Cht nh ho
5. Yu cu k thut
5.1. nh tnh
tan
t tan trong nc, tan trong ethanol.
Acid bo
ng
Phi c phn ng c trng ca ng.
5.2. tinh khit

Tro sulfat
Khng c qu 2%
Th 1 g mu (Phng php I)
Ch s acid
Khng c qu 6
Sucrose t do
Khng c qu 5% (m t trong phn Phng php th)
Dimethylformamid
Khng c qu 1,0 mg/kg (m t trong phn Phng

php th)
Dimethyl sulfoxid

php th)
Ethyl acetat,
isopropanol v
propylen glycol
Khng c qu 350,0 mg/kg, dng n cht hoc hp

cht (m t trong phn Phng php th)
Isobutanol

php th)
Methanol

php th)
Methyl ethyl keton

67
QCVN 4-22: 2011/BYT

php th
68
QCVN 4-22: 2011/BYT

Ch
5.3. Hm lng
Khng c nh hn 80,0% ester sucrose
6. Phng php th
6.1. nh tnh
Acid bo
Cho 1 ml ethanol vo 0,1 g mu, lm m v ho tan, thm

5 ml dung dch H2SO4 long TS, gia nhit trong cch thy
trong 30 pht v lm ngui. Cht c hoc du mu trng
vng c hnh thnh, khng c mi ca acid isobutyric v
c ho tan khi thm 3 ml diethyl ether. S dng lp
dung dch nc tch khi t diethyl ether cho Php th
ng.
ng
Cho vo 2 ml lp dung dch nc tch khi diethyl ether

trong php th acid bo, 1 ml anthron TS vo trong ng
th, cho cn thn theo thnh ng nghim; b mt ranh gii
gia hai lp chuyn thnh mu xanh da tri hoc xanh l
cy.
6.2. tinh khit
69
QCVN 4-22: 2011/BYT

Sucrose t do
Xc nh bng sc k kh lng (Quyn 4)

Dung dch chun:
Chun b dung dch gc cha 5 mg/ml sucrose trong N, Ndimethylformamid. Chun b mt lot cc dung dch chun
cha 0,5; 1,25 v 2,5 mg/ml sucrose bng cch pha long
dung dch gc vi pyridin.
Dung dch ni chun:
Cn chnh xc 0,25 g octacosan cho vo bnh nh mc
dung tch 50 ml, thm vo 25 ml tetrahydrofuran ho tan
octacosan, v nh mc n th tch 50 ml bng pyridin.
Cc iu kin sc k:
Ct: 2% Dexsil 300GC trn Uniport HP 80/100 mesh (t
phn cc, 2,1 m x 3.2 mm ng knh trong) hoc tng
ng
Kh mang: nitrogen
Detector: FID
Nhit :
- Bung bm mu: 2800C
- Ct: gi 1600C trong 1 pht sau tng t 160 n
3000C vi tc 150C/pht, gi trong 60 pht 3000C.
- Detector: 3200C
Thi gian lu ln lt ca sucrose v octacosan o c
vi cc iu kin trn xp x 8,2 v 9,8 pht.
Cch tin hnh: Cn chnh xc 20 50 mg mu cho vo
ng li tm, thm 1 ml dung dch ni chun, 1 ml pyridin, 0,4
ml N, O-bis (trimethylsilyl) acetamid (BSA) v 0,2 ml
trimethylchlorosilan (TMCS). Sau khi y np ng, lc v
yn trong 5 pht nhit phng. Bm 1l vo thit b
sc k kh lng.
ng chun:
Chun b dung dch chun silylat theo cch tin hnh nh
nhau s dng 1 ml mi loi dung dch chun thay th mu
v pyridin. V ng chun trn th lng sucrose (mg)
trong 1 ml dung dch chun (biu th trn trc X) so vi t l
din tch pic ca sucrose/ni chun (biu th trn trc Y).
o din tch pic i vi sucrose v ni chun. Tnh t l
din tch cc pic ca chng, v tnh c hm lng
sucrose trong mu da vo ng chun.
Lng sucrose pht hin c (mg)
% sucrose = ----------------------------------------------------- x 100
Khi lng mu (mg)
70
QCVN 4-22: 2011/BYT

Dimethylformamid
Dung dch chun:
Chun b dung dch gc cha 1 mg/ml dimethylformamid
trong tetrahydrofuran. Chun b mt lot cc dung dch
chun cha 0,05; 0,1 v 0,2 g/ml dimethylformamid bng
cch pha long dung dch gc vi tetrahydrofuran.
Cc iu kin sc k:
Ct: polyethylen glycol (di 30 m x 0,32 mm ng knh
trong vi dy lp phim mng 0,5 m)
Kh mang: heli
p sut: 150 kPa (p sut khng i)
Detector: detector nitrogen phosphor (NPD) [(tn khc:
Detector nhit ion ngn la (FTD)]
Nhit :
- Bung bm mu: 1800C
- Ct: gi 400C trong 2 pht sau tng t 40 n 160 0C
vi tc 200C/pht, gi trong 2 pht 1600C.
- Detector: 3250C
Phng php tim mu: Tim khng chia dng 1,0 l mu
bng bm t ng, sau bt u lm sch sau 1 pht.
Thi gian lu ca dimethylformamid o c vi cc iu
kin trn xp x 6,4 pht.
Cch tin hnh:
Cn chnh xc 2 g mu cho vo bnh nh mc dung tch
20 ml, thm vo 10 ml tetrahydrofuran ho tan mu,
thm tetrahydrofuran vo bnh n th tch 20 ml v lc
u dung dch. Bm 1,0 l dung dch mu vo thit b sc
k.
ng chun:
Chun b hng ngy bng cch bm 1,0 l mi dung dch
chun vo thit b sc k.
Tnh nng dimethylformamid (CDFA) theo cng thc sau:
Trong :
C: Nng dimethylformamid pht hin c (g/ml)
W: Khi lng mu (g)
Lu : Detector nitrogen phosphor khng nhy vi cc
thnh phn khng cha N hoc P. V th, ct mao qun c
th tc vi cc hp cht bay hi thp, mc d ng nn
ca sc k n nh. Do , ct phi c luyn thng
xuyn. Luyn qua m (dng kh mang theo hng ngc
1800C ) c thc hin sau khong mi t 15 mu.
71
QCVN 4-22: 2011/BYT

Dimethyl sulfoxid
Dung dch chun:
Chun b dung dch gc 0,25 mg/ml dimethyl sulfoxid trong
tetrahydrofuran. Chun b mt lot cc dung dch chun
cha 0,5; 1 v 5 g/ml dimethyl sulfoxid bng cch pha
long dung dch gc vi tetrahydrofuran.
Cc iu kin sc k:
Ct: 10% PEG 20M v 3% KOH trn Gas Chrom Z (chiu
di 2 m x 3 mm ng knh trong). Tng nhit l ti
1800C vi tc 100C/pht v n nh 24 48 gi vi
iu kin tc dng kh nitrogen 30 40 ml/pht luyn
ct.
Kh mang: nitrogen
Tc dng: 50 ml/pht
Detector: detector trc quang ngn la (s dng b lc lu
hunh 394 nm)
Nhit :
- Bung bm mu: 2100C
- Ct: 1600C.
Thi gian lu ca dimethyl sulfoxid o c vi cc iu
kin trn xp x 3,4 pht.
Cch tin hnh:
25 ml, thm vo 10 ml tetrahydrofuran ho tan mu,
thm tetrahydrofuran vo bnh n th tch 20 ml v lc
u dung dch. Bm 3 l dung dch mu vo thit b sc k.
ng chun:
Chun b hng ngy bng cch bm 3 l mi dung dch
chun vo thit b sc k.
Tnh nng dimethyl sulfoxid (CDMSO) theo cng thc sau:
Trong :
C: Nng dimethyl sulfoxid pht hin c (g/ml)
W: Khi lng mu (g)
72
QCVN 4-22: 2011/BYT

Propylen glycol
Dung dch ni chun:
Chun b dung dch 500 g/ml ca ethylen glycol trong
pyridin
Dung dch chun:
Chun b dung dch 50 g/ml ca propylen glycol trong
pyridin
Cc iu kin sc k:
Ct: Polydimethylsiloxan (chiu di 30 m x 0,32 mm ng
knh trong vi dy lp phim mng 0,25 m)
Kh mang: heli
Tc dng: 1,5 ml/pht (dng khng i)
Detector: FID
Nhit :
- Bung bm mu: 2300C
- Ct: gi 600C trong 5 pht sau tng t 60 n 250 0C
vi tc 200C/pht, gi trong 5 pht 2500C.
- Detector: 2500C
Thi gian lu ln lt ca dn xut ethylen glycol v dn
xut propylen glycol xp x 7,7 pht v 7,9 pht.
Cch tin hnh:
10 ml, thm vo 100 l dung dch ni chun. Ho tan v
nh mc n th tch 10 ml bng pyridin. Ly 0,5 ml dung
dch mu cho vo ng li tm, v thm 0,25 ml 1,1,1,3,3,3
hexamethyldisilazan (HMDS) v 0,1 ml trimethylchlorosilan
(TMCS). Sau khi y cht np ng, lc mnh, yn trong
30 pht nhit phng, sau li tm. Bm 1 l dung
dch ni trn mt ng sau li tm vo thit b sc k.
ng chun:
Tin hnh sc k nh trn, trong dng 0,05; 0,2; 0,5 v
1ml dung dch chun thay th cho dung dch mu th.
Tnh nng propylen glycol (CPG) theo cng thc sau:
Trong :
C: Nng propylen glycol pht hin c (g/ml)
W: Khi lng mu (g)
Lu : Nht thit phi lm sch cng bm mu v luyn
ct 3000C sau mi t 20 mu phn tch, bi ct b
nhim bn.
73
QCVN 4-22: 2011/BYT

Methanol, isopropanol,
isobutanol, ethyl
acetat v methyl
ethyl keton
Xc nh bng sc k kh c bung ly mu khng gian

hi.
Dung dch chun:
Chun b dung dch chun A cha 4.000 mg/l mi loi
methanol, isopropanol, isobutanol, ethyl acetat v methyl
ethyl keton bng cch cn chnh xc 0,2 g mi dung mi v
cho vo bnh nh mc dung tch 50 ml cha khong 20 ml
nc, sau thm nc vo n th tch 50 ml. Chun b
cc dung dch cha 2.000 mg/l (dung dch chun B) v 1.000
mg/l (dung dch chun C) bng cch pha long dung dch
chun A.
Cch tin hnh:
Cn chnh xc 4 g mu cho vo 4 l (mi l 1 g mu). Cho
5 l nc vo l th nht, cho ln lt vo l th hai, th
ba, th bn dung dch chun A, B v C; y nhanh septum.
(Nng ca mi dung mi sau khi thm 5 l dung dch
chun A, B, C vo 1 g mu tng ng ln lt bng 20,
10 v 5 mg/kg mu). l mu trong bung ly mu khng
gian hi v phn tch vi cc iu kin sau:
Ct: 100% Polydimethylsiloxan (chiu di 30 m x 0,53 mm
ng knh trong vi dy mng phim mng 1,5 m), v
d: DB 1 c sn xut bi Cng ty TNHH J & W)
Kh mang: nitrogen
Tc dng: 3,5 ml/pht
Detector: FID
Nhit :
- Bung bm mu: 1100C
- Ct: 400C.
- Detector: 1100C
Bung ly mu khng gian hi:
- Nhit cch nhit mu: 800C
- Thi k cch nhit mu: 40 pht
- Nhit syringe: 850C
- Bm mu dng kh: 1,0 ml
Kt qu:
th biu din mi tng quan gia lng thm vo vi
din tch pic i vi mi dung mi s dng cc kt qu
phn tch. Mi tng quan phi tuyn tnh (R 2 > 0,99).
Ngoi suy v xc nh x phn b chn, w i, v tnh nng
dung mi Ci (mg/kg) trong mu:
Trong :
wi: Phn b chn ca ng thng tng quan s dng
phng php thm chun (g)
74
QCVN 4-22: 2011/BYT

W: Khi lng mu (g)
75
QCVN 4-22: 2011/BYT

Ch

6.3. nh lng
Xc nh bng HPLC s dng cc iu kin sau:

Cch tin hnh:
Cn chnh xc 250 mg mu v cho vo bnh nh mc
dung tch 50 ml. Pha ti th tch 50 ml bng
tetrahydrofuran v lc u. Lc qua mng lc 0,5 m. Bm
100 l mu vo thit b sc k n nh trc.
Cc iu kin sc k:
Ct: Styren-divinylbenzen copolymer i vi sc k thm
thu qua gel (TSK-GEL G2000 (Tosoh) hoc tng ng)
Pha ng: tetrahydrofuran dng cho HPLC bi kh
Tc dng: 0,7 ml/pht
Detector: RI
Nhit :
- Ct: 380C.
- Detector: 380C
Ghi sc k trong khong 90 pht.
Tnh % ester sucrose trong mu:
% ester sucrose = 100 A/T
Trong :
A: Tng cc din tch pic i vi 3 thnh phn chnh,
mono-, di- v tri-ester, ra gii ln lt khong 65, 68 v
73 pht.
T: Tng din tch tt c cc pic ra gii trong khong 90
pht
76
QCVN 4-22: 2011/BYT

Ph lc 16
I VI DIOTYL NATRI SULFOSUCINAT
1. Tn khc, ch s
DSS, natri docusat,

INS 480
ADI = 0 - 0,1 mg/kg th trng
2. nh ngha
Tn ha hc
Natri1,4-bis-(2-ethylhexyl)-sulfosuccinat; Mui natri ca acid

ester sulfo-1,4-bis-(2-ethylhexyl) butanedioic; dioctyl natri
sulfosuccinat
S C.A.S.
577-11-7
Cng thc ha hc
C20H37NaO7S
Cng thc cu to
Khi lng phn t
444,56
3. Cm quan
Cht rn dng do, ging sp, mu trng c mi c trng

ging octanol, nhng khng c mi ca cc dung mi khc.
4. Chc nng
Cht nh ha, cht lm m
5. Yu cu k thut
5.1. nh tnh
tan
t tan trong nc, d tan trong ethanol v glycerol
Ph hng ngoi
Ph hng ngoi ca mu phn tn trong kali bromid tng

ng vi ph ca mu chun i chiu (Chun i chiu
USP dioctyl sulfosuccinate c cng ty United States
Pharmacopoeia, 12601 Twinbrook Parkway, Rockville, Md
20852, USA)
pH
5.8 - 6.9 (dung dch 1/100)
5.2. tinh khit

Gim khi lng khi lm
kh
Khng c qu 2 % (105C trong 2 gi)
trong ca dung dch
Ha tan 25 g mu th vo 94 ml ethanol. Dung dch khng

c vn c sau 24 gi.
Tro sulfat
Trong khong t 15,5 % n 16,2 %.

77
QCVN 4-22: 2011/BYT

(th theo hng dn ti JECFA monograph 1 - Vol.4;
Phng php I, cn 1 g mu)
78
QCVN 4-22: 2011/BYT

Bis-(2-ethylhexyl)-maleat
Khng c qu 0,4 %.
Ch
5.3. Hm lng
Khng thp hn 98,5 % tnh theo khi lng kh.
6. Phng php th
6.1. tinh khit
Bis-(2-ethylhexyl)-maleat
Thuc th
- Cht in gii h tr: Ha tan 21,2 g lithi perchlorat
(LiClO4) khan vo 175 ml nc trong cc 250 ml. iu
chnh pH ca dung dch ny n 3,0 bng cch thm tng
git acid acetic bng (khong 1 n 2 git l ), dng mt
my o pH ph hp. Chuyn ton lng dung dch vo
bnh nh mc 200 ml, pha long n vch bng nc, v
trn u.
- Dung dch chun: Chuyn 100 - 110 mg (cn chnh xc)
bis-(2-ethyl-hexyl)-maleat, (bis-(2-ethylhexyl)-maleat vi
tinh khit ph hp c tn khc l OT-35 ca Cng ty
American Cyanamid, Pine Chemicals Department, Pearl
River, New York 10965, USA), vo bnh 100 ml. Ghi li khi
lng chnh xc, chnh xc n 0,1 mg, Wa. Pha long n
vch bng nc, trn u.
- Dung dch mu th gc: Chuyn 12,5 g mu th,
c cn chnh xc, vo cc 150 ml. Ghi li khi lng
chnh xc, Ws, chnh xc n 10 mg. Thm 80-90 ml
isopropanol, khuy bng a thy tinh n khi mu tan
hon ton. Chuyn ton lng dung dch ny vo bnh nh
mc 250 ml bng isopropanol. Pha long n vch bng
isopropanol, trn u.
- Dung dch th A: Dng pipet ly 50.0 ml "Dung dch mu
th gc" v 20,0 ml "Dung dch in gii h tr " vo bnh
nh mc 100 ml. Pha long vi isopropanol n khong
di vch nh mc 15 mm, y nt, lc u v trong 2
pht. Pha long tip bng isopropanol n vch, y nt,
lc u. Phi thu c dung dch tuyt i trong.
- Dung dch th B: Dng pipet ly 50,0 ml "Dung dch mu
th gc", 10,0 ml "Dung dch chun", v 20,0 ml Dung
dch in gii h tr" vo bnh nh mc 100 ml, v tip tc
qui trnh nh miu t trong phn Dung dch th A
- Mu trng: Dng pipet ly 20,0 ml "Dung dch in gii h
tr" vo bnh nh mc 100-ml, pha long n vch bng
isopropanol, trn u.
Tin hnh
Ra bnh cc ph H-cell vi ln bng tng lng nh
Dung dch th A, sau y mt na bnh bng dung
dch ny, t mt mu giy thm ln ming bnh v cho
dng kh nitrogen chy t t qua dung dch trong 15 pht
(Ch : Trc ht phi bo ha nitrogen bng cch cho
chy qua bnh sc ph hp c cha isopropanol). Sau 15
79
QCVN 4-22: 2011/BYT

pht, hng dng nitrogen ln b mt dung dch v ly giy
ra khi bnh. Vi mt cc ph k ph hp c hiu
chun trc (nh cc ph k Metrohm Polacord E-261,
hoc tng ng t mt th phn cc -1,3V. iu
chnh nhy dng ti thang thp nht (nhy nht) m ti
cc dao dng dng vn nm trong thang. Ghi li cc
ph ti nhy ny, qut th trong khong t -0,9 n
-1,5 V, dng in cc so snh l in cc calomel bo ha.
Ghi li dao ng trung bnh A ti th -1,3 V, v dao ng
trung bnh B, ti th -1,0 V, theo mm. (Ch : nu s dng
cc ph k khng t ng, ghi li cc dao ng dng
khuch tn trung bnh ca dung dch tng ng ti -1,3 V
v -1,0V). Lp li ton b qu trnh vi dung dch th B, ghi
li gi tr dao ng dng khuch tn trung bnh, D, ti -1,3 V
v E, ti -1,0 V.
Lm tng t vi mu trng, ghi li gi tr dao ng dng
khuch tn trung bnh, G, ti -1,3V v H, ti -1 V.
Tnh ton:
Trc ht tnh cc ga tr sau (theo mA):
trong
C l cng dng khuch tn ca Dung dch th A v
S1 l nhy dng khi o "Dung dch th A"
trong
F l cng khuch tn ca Dung dch th B v
S2 l nhy dng khi o "Dung dch th B"
trong
I l cng dng khuch tn ca Mu trng v
S3 l nhy dng khi o "Mu trng"
trong
J l dng khuch tn gy ra do thm maleat t Dung dch
chun vo Dung dch th B.
trong
K dng khuch tn gy ra do maleat c trong Dung dch th
A.
Cui cng, tnh phn trm ca bis-(2-ethylhexyl)-maleat c
trong mu ban u theo cng thc sau:
80
QCVN 4-22: 2011/BYT

Ch

6.2. nh lng
Cc dung dch
- Dung dch mu: Chuyn khong 3,8 g mu th, trc
c sy kh 105C trong 2 gi v c cn
chnh xc, vo bnh nh mc 500 ml, ha tan trong
cloroform. Pha long n vch bng dung mi trn, trn
u.
- Dung dch tetra-n-butylamoni iodid: Chuyn 1,250 g tetran-butylamoni iodid vo bnh nh mc 500 ml, pha long
n vch bng nc, trn u.
- Dung dch mui: Ha tan 100 g natri sulfat khan v 10 g
natri carbonat vo mt lng nc va c c th
tch cui cng l 1000 ml.
Tin hnh
Dng pipet ly 10,0 ml "Dung dch mu" vo bnh nh mc
250 ml, thm vo 40 ml cloroform, 50 ml "Dung dch
mui", 10 git dunh dch xanh bromophenol (TS). Chun
bng "Dung dch tetra-n-butylamoni iodid" n khi bt
u xut hin mu xanh trong lp cloroform sau khi lc
mnh dung dch. Tnh hm lng (%) C20H37NaO7S theo
cng thc:
trong
V = th tch (ml) ca dung dch tetra-n-butylamoni iodid
dng chun .
444,6 = khi lng phn t ca dioctyl natri sulfosuccinat
W = khi lng (g) ca mu th
369,4 = khi lng phn t ca tetra-n-butylamoni iodid.
81
QCVN 4-22: 2011/BYT

Ph lc 17
I VI STEARYL TARTRAT
1. Tn khc, ch s
2. nh ngha
Tn ho hc
Cng thc ho hc
Stearyl palmityl tartrat;

INS 483
Sn phm ca qu trnh ester ho acid tartric vi
cn stearylic thng mi, v c bn gm cn
stearylic v palmitylic; gm thnh phn chnh l
diester, vi lng nh monoester v cc nguyn
liu ban u khng thay i.
Cc thnh phn chnh l distearyl tartrat, dipalmityl
tartrat v stearylpalmityl tartrat.
Distearyl tartrat: C40H78O6
Dipalmityl tartrat: C36H70O6
Stearylpalmityl tartrat: C38H74O6
Cng thc cu to
Khi lng phn t
Trong R l (CH2)17CH3 hoc (CH2)15CH3

Distearyl tartrat: 655,06
Dipalmityl tartrat: 598,95
Stearylpalmityl tartrat: 627
3. Cm quan
Cht nhn c mu kem
4. Chc nng
Cht nh ha, cht x l bt
5. Yu cu k thut
5.1. nh tnh
tan
Khng tan trong nc, khng tan trong ethanol lnh, tan
trong ethanol nng.
Nhit nng chy
67 770C
Ch s hydroxyl
200 220
Tartrat
Phi c phn ng c trng ca tartrat.
5.2. tinh khit

Tro sulfat
Khng c qu 0,5% (Th trn 2 g mu, phng php I )
Acid tartric tng s
Khng c nh hn 18% v khng c qu 35% (m t

trong phn Phng php th)
Cht khng x phng

ha
Khng c nh hn 77% v khng c qu 83% (m t

trong phn Phng php th)
82
QCVN 4-22: 2011/BYT

Ch s acid
Khng c qu 6 (m t trong phn Phng php th)
Ch
5.3. Hm lng
Khng c nh hn 90% hm lng ester tng s tng

ng vi ch s ester trong khong 163 180.
6. Phng php th
6.1. tinh khit
Acid tartric tng s
ng chun:
Cn 100 mg acid tartric tinh khit cho vo bnh nh mc
dung tch 100 ml, ho tan trong khong 90 ml nc, thm
nc vo cho n khi t th tch 100 ml v lc u.
Chuyn cc phn tch bit 3, 4, 5, 6 ml vo trong cc cuvet
ph hp 19 x 150 mm, thm lng nc va n 10
ml. Thm vo 4 ml dung dch natri metavanadat 5% va
chun b v 1 ml acid acetic vo mi cuvet. (Ch : s
dng cc dung dch ny trong 10 pht sau khi xut hin
mu). Chun b mu trng theo cch tng t, s dng 10
ml nc thay th dung dch acid tartric. t trn thit b
hp th bng 0 i vi mu trng, sau o hp th
ca 4 dung dch acid tartric bc sng 520 nm vi my
quang ph thch hp hoc my so mu quang in c
trang b knh lc 520 nm. T cc kt qu thu c, v
ng chun trn h to vung gc vi trc tung biu
din hp th v trc honh biu din hm lng acid
tartric (mg).
Chun b mu th:
Cn chnh xc 4 g mu cho vo bnh tam gic dung tch
250 ml v thm vo 80 ml dung dch KOH 0,5N v 0,5 ml
phenolphthalein TS. Ni bnh vi mt sinh hn khng kh
c chiu di t nht 65 cm v gia nhit hn hp trn tm
bn nng trong 2,5 gi. Thm vo hn hp nng acid
phosphoric 10% cho n khi c phn ng acid r rt pht
hin c bng giy th congo. Li kt ni sinh hn kh
v gia nhit cho n khi acid bo ho lng v trong. Lm
ngui v chuyn hn hp vo mt phu chit dung tch 250
ml bng cc phn nh nc v chloroform. Chit tch cc
acid bo c gii phng ra bng 3 ln lin tip 25 ml
nc v cho phn nc ra vo phu chit cha lp
nc. Chuyn cc thnh phn c trong phu chit th nht
vo cc 250 ml, gia nhit trn chu hi nc loi cc
vt chloroform, lc qua giy lc mn vo bnh nh mc
dung tch 500 ml v cui cng pha ti th tch 500 ml bng
nc (Dung dch I). Dng pipet ly 25 ml dung dch ny
cho vo bnh nh mc dung tch 100 ml v pha ti th tch
100 ml bng nc (Dung dch II).
Cch tin hnh:
Chuyn 10 ml Dung dch II c chun b trong phn
Chun b mu th vo cuvet 19 x 150. Thm vo 4 ml dung
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QCVN 4-22: 2011/BYT

dch natri metavanadat 5% va chun b v 1 ml acid
acetic. (Ch : s dng cc dung dch ny trong 10 pht
sau khi xut hin mu). Chun b mu trng theo cch
tng t, s dng 10 ml nc thay th dung dch acid
tartric. t trn thit b o hp th bng 0 i vi mu
trng, sau o hp th ca 4 dung dch acid tartric
bc sng 520 nm vi my quang ph thch hp hoc my
so mu quang in c trang b knh lc 520 nm. T
ng chun xc nh hm lng acid tartric (mg) trong
dung dch pha cui cng, nhn hm lng acid tartric xc
nh c vi 20 v chia cho trng lng mu ban u
thu c % acid tartric.
84
QCVN 4-22: 2011/BYT

Cht khng x phng
ha
Cch tin hnh ny xc nh nhng cht ha tan trong cht

bo m khng c x phng ho bi kim nhng c
ha tan trong dung mi cht bo thng thng.
Cch tin hnh:
Cn chnh xc 5 g mu cho vo bnh dung tch 250 ml,
thm dung dch c 2 g KOH trong 40 ml alcol v un si
nh c sinh hn ngc trong 1 gi. Chuyn ton b hn
hp cha trong bnh vo ng ong c np y thu tinh
(chiu cao khong 30 cm, ng knh 3,5 cm v c vch
nh mc 40, 80 v 130 ml). Ra bnh bng alcol ph hp
n th tch 40 ml trong ng ong, thm nc m, sau
bng nc lnh cho n khi tng th tch t 80 ml. Cui
cng ra bnh bng vi ml ether du ha, cho phn dung
mi ra vo ng ong, lm mt hn hp trong ng ong
n nhit phng v thm 50 ml ether du ha.
y np, lc ng ong mnh t nht trong 1 pht, hai
lp tch ra trong. Ht lp bn trn hon ton nu c th
m khng ht bt k mt cht dch no ca lp di, ly
phn ether cho vo trong mt phu tch dung tch 500 ml.
Lp li qu trnh trch ly v ht dch t nht 6 ln bng cc
phn 50 ml ether du ha, lc mnh mi ln. Ra hn hp
phn trch ly bng cc phn 25 ml alcol 10% v lc mnh
cho n khi nc ra c trung ho s dng cht ch th
phenolphthalein, v loi b phn nc ra. Chuyn phn
ether tch c vo cc bit khi lng v ra phu
tch bng 10 ml ether, sau cho nc ra vo cc.
C ether trong cch thy n kh v lm kh phn cn n
khi lng khng i, tt nht 75 80 0C p sut chn
khng khng qu 200 mm Hg, hoc 100 0C p sut
thng trong 30 pht. Lm mt trong bnh ht m v cn
thu c khi lng cha hiu chnh ca cht khng x
phng.
Xc nh hm lng acid bo trong cn bng cch sau:
Ho tan cn trong 50 ml alcol m (cha phenolphthalein
TS v trc c trung ho bng NaOH ti mu hng
nht), chun bng dung dch NaOH 0,02N cho n khi
xut hin mu hng nht. Mi ml dung dch NaOH 0,02N
tng ng vi 5,659 mg acid bo, tnh theo acid oleic.
Hiu s khi lng cha hiu chnh ca cht khng x
phng v khi lng acid bo tnh c t php chun
trn l khi lng cht khng x phng ha trong mu th.
85
QCVN 4-22: 2011/BYT

Ch s acid
Cn chnh xc 1 g mu v ho tan trong 20 ml ethanol 95%

nng, trc c trung ho c s dng 0,5 ml cht
ch th phenolphthalein TS. Lm ngui dung dch sau
trung ho bng cch chun vi dung dch KOH 0,01N
trong ethanol.
0,561 x th tch dung dch KOH dng
chun (ml)
Ch s acid =
-----------------------------------------------------------------------Khi lng mu (g)
Gi li dung dch c trung ho cho phn nh lng.
Ch

6.2. nh lng
Thm chnh xc 50 ml dung dch KOH 0,1N trong ethanol

vo dung dch c trung ho trn t phn xc nh
ch s acid v un si u trong 2 pht. Lm ngui dung
dch v chun d KOH bng B ml dung dch HCl 0,1N.
Thc hin xc nh vi mu trng ( bng A ml dung dch
HCl 0,1N).
5,611 x (A B)
Ch s ester = ----------------------------------------Khi lng mu (g)
86
QCVN 4-22: 2011/BYT

Ph lc 18
I VI SORBITAL MONOSTEARAT
1. Tn khc, ch s
INS 491
ADI=0-25mg/kg th trng
2. nh ngha
Hn hp bao gm cc ester mt phn ca sorbitol v cc

dn cht mono- v dianhydrid ca n vi acid stearic thc
phm.
Ch s C.A.S
1338-41-6
Cng thc cu to
Gm acid palmitic este ha vi polyol dn xut t sorbitol

bao gm cc loi sau:
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
Ht hay mnh c mu kem nht n vng nu hoc dng

sp rn, c mi nh c trng.
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
Ti nhit cao hn im chy, tan trong toluen, dioxan,

carbon tetraclorid, ether, methanol, ethanolv anilin; khng
tan trong ether du ha v aceton, khng tan trong nc
lnh nhng c th phn tn trong nc m.Ti nhit
trn 50oC tan dng sng m trong du khong v ethyl
acetat.
Khong nhit ng
c
50-52oC.
Hp th hng ngoi
Ph hng ngoi ca mu th c trng cho este mt phn

ca acid bo vi polyol
5.2. tinh khit

Nc
Khng c qu 1,5% (phng php Karl Fischer).
Ch s acid
Khng c thp hn 5 v khng c qu 10.
Ch s x phng ha
87
QCVN 4-22: 2011/BYT

Ch s Hydroxyl
Ch
5.3. Hm lng
X phng ha 100g mu phi thu c khong 31,5g

polyol v 73g acid bo. Hm lng polyol khng c thp
hn 95% trong hn hp sorbitol, 1,4-sorbitan v isosorbid.
6. Phng php th
6.1. tinh khit
Ch

6.2. nh lng
Tin hnh theo hng dn trong chuyn lun xc nh

hm lng sorbitan ester (JECFA monograph 1 - Vol.4 ).
88
QCVN 4-22: 2011/BYT

Ph lc 19
I VI SORBITAN TRISTEARAT
1. Tn khc, ch s
INS 492
2. nh ngha

dn cht mono- v dianhydrid ca n vi acid stearic thc
phm.
Ch s C.A.S
26658-19-5
Cng thc cu to
Gm acid stearic este ha vi polyol dn xut t sorbitol

bao gm cc loi sau:
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
Ht hay mnh c mu kem nht n vng nu hoc dng

sp rn
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
Kh tan trong toluen, ether, carbon tetraclorid, ethyl acetat;

c th phn tn trong ether du ho, du khong, du thc
vt, aceton v dioxan; khng tan trong nc, methanol v
ethanol (th theo hng dn ti JECFA monograph 1 Vol.4 ).
Khong nhit ng
c
47-50oC.
5.2. tinh khit

Nc
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 15.
Ch s x phng ha
Ch s Hydroxyl
89
QCVN 4-22: 2011/BYT

Ch
5.3. Hm lng
X phng ha 100g mu phi thu c khng thp hn

14g v khng c qu 21g polyol v khng thp hn 85g
v khng c qu 92g acid bo. Hm lng polyol khng
c thp hn 95% trong hn hp sorbitol, 1,4-sorbitan v
isosorbid.
6. Phng php th
6.1. tinh khit
Ch
6.2. nh lng

thch hp cho hm lng quy nh. La chn c mu th v
Cn 25g mu th, chnh xc n mg, chuyn vo bnh cu
y trn 500 ml, thm 250 ml cn v 7,5g kali hydroxyd v
trn u. Lp bnh cu vi sinh hn thch hp, un hi lu
hn hp trong t 1-2 gi sau chuyn hn hp sang cc
800 ml, trng sch bnh bng 100 ml nc ct v gp dch
ra vo cc. Cho bay hi ht cn trn b cch thu, thnh
thong thm nc thay th lng cn bay hi. Dng
qu trnh ui cn khi khng cn mi cn bay ra. Hiu
chnh th tch cui cng cho 250 ml bng nc nng.
Trung ho dung dch x phng vi acid sulfuric long (1/2),
thm 10% d v un nng, khuy u cho n khi acid bo
tch lp. Chuyn lp acid bo sang phu chit 500 ml, ra
3 hoc 4 ln, mi ln vi 20 ml nc nng loi ht cc
polyol, gp dch ra vi pha nc cha polyol thu c t
qu trnh x phng ho. Chit pha nc ny 3 ln 20 ml
ether du ho/ln, ly lp ether du ho gp vi phn acid
bo, cho bay hi ti kh trong mt a xc nh b,
ngui v cn.
Trung ho dung dch cha polyol bng dung dch kali
hydroxyd 1/10 ti pH = 7, s dng pH k thch hp. Cho
bay hi dung dch ny ti gn cn, tch phn polyol khi
cc mui bng cch chit vi ln vi cn nng. Cho bay hi
dch chit cn trn b cch thu ti kh trong mt a
xc nh b, ngui v cn. Trnh kh qu trong qu trnh
un nng.
Tin hnh nh lng mt mu khc (25g) theo hng dn
chuyn lun xc nh hm lng ester sorbitan xc nh
% ester sorbitan.
90
QCVN 4-22: 2011/BYT

Ph lc 20
I VI SORBITAN MONOLAURAT
1. Tn khc, ch s
INS 493
2. nh ngha

dn cht mono- v dianhydrid ca n vi acid lauric thc
phm.
Ch s C.A.S
1338-39-2
Cng thc cu to
Gm acid lauric este ha vi polyol dn xut t sorbitol bao

gm cc loi sau:
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
Dng lng nht snh c mu h phch, dng ht hay mnh

c mu kem nht n vng nu hoc dng sp rn, c mi
nh c trng.
4. Chc nng
Cht nh ha, cht n nh
5. Yu cu k thut
5.1. nh tnh
tan
C th phn tn c trong nc nng v nc lnh.
5.2. tinh khit

Nc
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 7.
Ch s x phng ha
Ch s Hydroxyl
Ch
5.3. Hm lng

36g v khng c qu 49g polyol, khng thp hn 56g
v khng c qu 68g acid bo. Hm lng polyol khng
c thp hn 95% trong hn hp sorbitol,
1,4sorbitan v isosorbid.
91
QCVN 4-22: 2011/BYT

6. Phng php th
6.1. tinh khit
Ch

6.2. nh lng

ngui v cn.
un nng.
92
QCVN 4-22: 2011/BYT

Ph lc 21
I VI SORBITAN MONOOLEAT
1. Tn khc, ch s
INS 494
2. nh ngha

dn cht mono- v dianhydrid ca n vi acid oleic thc
phm (R). Thnh phn ln nht l 1,4-Sorbitan monooleat,
thnh phn t hn l isosorbid monooleat, sorbitan dioleat
v sorbitan trioleat.
Ch s C.A.S
1338-43-8
Cng thc cu to
Gm acid oleic este ha vi polyol dn xut t sorbitol bao

gm cc loi sau:
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
Dng st snh mu h phch, dng ht hay mnh c mu

kem nht n vng nu hoc dng sp rn, c mi nh .
4. Chc nng
Cht nh ha, cht n nh
5. Yu cu k thut
5.1. nh tnh
tan
Ti nhit cao hn im chy, tan trong ethanol, ether,

ethylacetat, anilin, toluen, dioxan, ether du ha, carbon
tetraclorid; khng tan trong nc lnh nhng c th phn
tn trong nc m.
Ch s iod
Phn acid oleic thu c bng cch x phng ho sorbitan

monooleat trong qu trnh nh lng c ch s iod t 80
n 100.
5.2. tinh khit

Nc
Khng c qu 2% (phng php Karl Fischer).
Tro sulfat
Khng c qu 0,5%.
Ch s acid
Khng c qu 8.
Ch s x phng ha
Ch s Hydroxyl

93
QCVN 4-22: 2011/BYT

Ch
Khng c qu 2,0 mg/kg
5.3. Hm lng

28g v khng c qu 32g polyol, khng thp hn 73g v
khng c qu 77g acid bo. Hm lng polyol khng
c thp hn 95% trong hn hp sorbitol, 1,4-sorbitan v
isosorbid.
6. Phng php th
6.1. tinh khit
Ch

6.2. nh lng

ngui v cn.
un nng.
Tin hnh nh lng mt mu khc (25g) theo hng dn
chuyn lun xc nh hm lng sorbitan ester xc nh
% sorbitan ester.
94
QCVN 4-22: 2011/BYT

Ph lc 22
I VI SORBITAN MONOPALMITAT
1. Tn khc, ch s
INS 495
2. nh ngha

dn cht mono- v dianhydrid ca n vi acid palmitic thc
phm
Ch s C.A.S
26266-57-9
Cng thc cu to
Gm acid palmitic ester ha vi polyol dn xut t sorbitol

bao gm cc loi sau:
Sorbitol
1,4-Sorbitan
Isosorbid
3. Cm quan
Dng sp rn c mu kem nht n vng nu, c mi nh .
4. Chc nng
Cht nh ha
5. Yu cu k thut
5.1. nh tnh
tan
Ti nhit cao hn im chy, tan trong methanol, ether,

ethylacetat, anilin, toluen, dioxan, ether du ha, carbon
tetraclorid; khng tan trong nc lnh nhng c th phn
tn trong nc m.
ng c
45 - 470
Hp th hng ngoi
Phi c ph hng ngoi c trng ca ester ca acid bo

vi polyol
5.2. tinh khit

Nc
Ch s acid
Khng c thp hn 4 v khng c jqu 7,5.
Ch s x phng ha
Ch s Hydroxyl
Ch
Khng c qu 2,0 mg/kg
5.3. Hm lng
X phng ha 100g mu phi thu c khong 37 g polyol

v 65 g acid bo. Hm lng polyol phi vo khong 95%
95
QCVN 4-22: 2011/BYT

trong hn hp sorbitol, 1,4-sorbitan v isosorbid.
6. Phng php th
6.1. tinh khit
Ch

6.2. nh lng
Tin hnh theo hng dn trong chuyn lun xc nh hm

lng sorbitan ester (JECFA monograph 1 - Vol.4 ).
96

Chat Nhu Hoa

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QCVN 4-22:2011/BYT

QUY CHUN K THUT QUC GIA

QCVN 4-22: 2011/BYT

Yu cu k thut v phng php th i vi monov di-glycerid ca acid bo

QCVN 4-22: 2011/BYT

2. Cc yu cu k thut quy nh trong Quy chun ny c th theo JECFA

3. Ly mu theo hng dn ti Thng t 16/2009/TT-BKHCN ngy 02 thng 6

QCVN 4-22: 2011/BYT

QCVN 4-22: 2011/BYT

Glyceryl monostearate, glyceryl monopalmitate, glyceryl

Hn hp cc ester mono- v diglyceryl mch di vi cc acid

Trong OCR l ca acid bo

Glyceryl monostearat: 358,6

Cht bo rn dng sp c mu trng hoc kem hoc dng

Khng tan trong nc, tan trong ethanol, cloroform v

Phi c ph hng ngoi c trng ca ester mt phn ca

Phi c phn ng c trng ca glycerol.

5.2. tinh khit

Khng c qu 2,0 % (phng php Karl Fischer)

QCVN 4-22: 2011/BYT

Khng c qu 6%, tnh theo natri oleat.

Khng c qu 2,0 mg/kg.

Thm 10 g mu th vo hn hp gm 60 ml aceton v 0,15

- Th theo JECFA monograph 1 - Vol.4.

QCVN 4-22: 2011/BYT

Lactic acid esters of mono- and diglycerides; lactoglycerides

L hn hp cc ester ca glycerol vi acid lactic v acid bo

Trong R1, R2 v R3 l ca acid bo, acid lactic hoc

Khng tan trong nc lnh nhng c th phn tn trong nc

Phi c phn ng c trng ca acid bo.

Phi c phn ng c trng ca acid lactic.

5.2. tinh khit

Ch c acid bo v acid lactic.

Khng c qu 2,0 mg/kg.

- Th theo JECFA monograph 1 - Vol.4.

QCVN 4-22: 2011/BYT

Citric acid esters of mono- and di-glycerides, citroglycerides,

Thu c nh qu trnh ester ho glycerol vi acid citric v

Trong : t nht mt trong R 1, R2 hoc R3 l ca acid citric,

Dng du ti sp, mu trng n trng ng

Cht n nh, cht nh ho, cht chng oxy ho

Khng tan trong nc lnh, c th phn tn trong nc

Phi c phn ng c trng ca acid bo .

Phi c phn ng c trng ca acid citric.

5.2. tinh khit

Sn phm khng c trung ho : Khng c qu 0,5%

8 33% (m t trong phn Phng php th)

Acid citric tng s

13 50% (m t trong phn Phng php th)

37 81% (m t trong phn Phng php th)

QCVN 4-22: 2011/BYT

Khng c qu 2,0 mg/kg.

Cn chnh xc 2 g mu v cho vo bnh x phng ho, thm

Acid citric tng s

QCVN 4-22: 2011/BYT

QCVN 4-22: 2011/BYT

W: Khi lng (g) ca mu ester glycerol vi acid citric v

QCVN 4-22: 2011/BYT

Diacetyltartric acid esters of mono- and diglycerides,

Sn phm gm hn hp cc ester ca glycerol vi acid

Cc thnh phn chnh l:

T dng lng, bt nho n dng rn ging sp (vy hoc

QCVN 4-22: 2011/BYT

Phn tn trong nc nng v nc lnh, tan trong methanol