CNG HA X HI CH NGHA VIT NAM

QCVN 4-6 : 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT CHNG OXY HA
National technical regulation
on Food additives Antioxidant agents

H NI - 2010

Li ni u
QCVN 4-6:2010/BYT do Ban son tho quy chun k thut
quc gia v Ph gia thc phm v cht h tr ch bin
bin son, Cc An ton v sinh thc phm trnh duyt v
c ban hnh theo Thng t s 23/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT CHNG OXY HA
National technical regulation on Food additives Antioxidant agents
1. 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 chng oxy 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 chng oxy 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 chng oxy ha: l ph gia thc phm c s dng vi mc ch
chng li s h hng ca thc phm do b oxy ha (nh i kht ca m, thay i
mu sc) nhm ko di thi hn s dng ca thc phm.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food addiditive 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. INS (International numbering system): H thng m s quc t v ph gia
thc phm.
II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht chng oxy ha c
quy nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1. Ph lc 1: Yu cu k thut v phng php th i vi acid ascorbic.

1.2. Ph lc 2: Yu cu k thut v phng php th i vi natri ascorbat.

1.3. Ph lc 3: Yu cu k thut v phng php th i vi calci ascorbat.
1.4. Ph lc 4: Yu cu k thut v phng php th i vi ascorbyl palmitat.
1.5. Ph lc 5: Yu cu k thut v phng php th i vi ascorbyl stearat.
1.6. Ph lc 6: Yu cu k thut v phng php th i vi acid erythorbic.
1.7. Ph lc 7: Yu cu k thut v phng php th i vi dl--tocopherol.
1.8. Ph lc 8: Yu cu k thut v phng php th i vi propyl galat.
1.9. Ph lc 9: Yu cu k thut v phng php th i vi nha gaiac.
1.10. Ph lc 10: Yu cu k thut v phng php th i vi tertbutylhydroquinon.
1.11. Ph lc 11: Yu cu k thut v phng php th i vi
butylhydroxyanisol.
1.12. Ph lc 12: Yu cu k thut v phng php th i vi
butylhydroxytoluen.
1.13. Ph lc 13: Quy nh k thut v phng php th i vi dilauryl
thiodipropionat.
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 chng oxy 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 chng oxy ha

Vic kim tra cht lng, v sinh an ton i vi cc cht chng oxy 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 chng oxy 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.
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.

Ph lc 1
YU CU K THUT V PHNG PHP TH I VI ACID ASCORBIC
1. Tn khc, ch s

Vitamin C
INS 300
ADI khng gii hn

2. nh ngha
Tn ha hc

L-ascorbic acid; ascorbic acid; 2,3-didehydro-L-threohexono-1,4-lacton; 3-keto-L-gulouranolacton

M s C.A.S.

50-81-7

Cng thc phn t

C6H8O6

Cng thc cu to

CH2 OH
H C OH
O
O
H
HO

OH

Khi lng phn t

176,13

3. Cm quan

Bt tinh th trng hoc hi vng, khng mi, im nng

chy khong 190 oC km theo phn hy.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, t tan trong ethanol, khng tan trong

ether.

Phn ng mu

t yu cu (m t trong phn phng php th).

Phn ng kh

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 0,4%.

Gc quay cc ring

[ ]D25 trong khong +20,50 v +21,5o.

pH

2,4 2,8 (Dung dch 1/50).

Tro sulfat

Khng c qu 0,1%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C6H8O6

Khng thp hn 99,0% tnh theo ch phm lm kh.

6. Phng php th
6.1. nh tnh
Phn ng mu

Ly 2 ml dung dch mu th 2,0% trong nc, thm 2 ml

nc, 0,1 g natri hydrocarbonat v khong 0,02 g st II
sulfat . Lc u v yn. Dung dch s c mu tm m,
mu tm s mt khi thm 5 ml dung dch acid sulfuric
long (TS).

Phn ng kh

Dung dch mu th trong nc s kh ngay dung dch

kali permanganat (TS) m khng cn un nng, sn
phm thu c l kt ta mu nu.
Dung dch mu th trong cn s lm mt mu ca dung
dch 2,6-diclorophenol indophenol (TS).

6.2. tinh khit

Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol. 4

- Lm kh trn acid sulfuric trong chn khng, trong 24
gi.

Ch

- Th theo hng dn ti JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn 0,4 g (chnh xc n mg) mu th c lm kh

trong bnh ht m mi trng chn khng trn acid
sulfuric trong 24 gi, ha tan trong 100 ml nc khng c
carbon dioxyd v 25 ml dung dch acid sulfuric long (TS).
Chun dung dch ny vi dung dch iod 0,1 N, khi gn
t im kt thc chun thm ch th l vi git dung
dch h tinh bt (TS) v chun tip n khi t im
kt thc.
Mi ml dung dch iod 0,1 N tng ng vi 8,806 mg
C6H8O6.

Ph lc 2
YU CU K THUT V PHNG PHP TH I VI NATRI ASCORBAT
1. Tn khc, ch s

INS 301
ADI khng gii hn

2. nh ngha
Tn ha hc

Natri L-ascorbat; Natri ascorbat; Natri 2,3-didehydro-Lthreo-hexono-1,4-lacton enolat; Natri 3-keto-Lgulofuranolacton enolat.

M s C.A.S.

134-03-2

Cng thc phn t

C6H7O6Na

Cng thc cu to

CH2OH
H C OH
O
O

Na+

H
-

OH

Khi lng phn t

198,11

3. Cm quan

Bt tinh th trng hoc gn nh trng, khng mi, s b

sm mu khi ngoi nh sng.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, tan rt t trong ethanol.

Ascorbat

Phi c phn ng c trng ca ascorbat.

Natri

Phi c phn ng c trng ca natri.

Phn ng kh

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 0,25%.

Gc quay cc ring

Dung dch mu th trong nc nng 10% (kl/tt) c [ ]D25

trong khong +1030 v +108o.

pH

6,5 - 8,0 (Dung dch 1/10).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C6H7O6Na

Khng thp hn 99,0% tnh theo ch phm lm kh.

6. Phng php th
6.1. nh tnh
Natri

- Th theo JECFA monograph 1 - Vol. 4

- Chun b dch th: nung mu th, acid ha cn bng
dung dch acid acetic long (TS), lc nu cn.

Phn ng kh

Dung dch mu th s lm mt mu ca dung dch 2,6diclorophenol indophenol (TS).

6.2. tinh khit

Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol. 4

- Lm kh:trn acid sulfuric trong bnh chn khng, trong 24
gi.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn 0,4 g (chnh xc n mg) mu th c lm kh,

ha tan trong 100 ml nc khng c carbon dioxyd v 25
ml dung dch acid sulfuric long (TS). Chun dung dch
ny vi dung dch iod 0,1 N, khi gn t im kt thc
chun thm ch th l vi git dung dch h tinh bt (TS)
v chun tip n khi t im kt thc.
Mi ml dung dch iod 0,1 N tng ng vi 9,905 mg
C6H7O6Na.

Ph lc 3
YU CU K THUT V PHNG PHP TH I VI CALCI ASCORBAT
1. Tn khc, ch s

INS 302
ADI khng gii hn

2. nh ngha
Tn ha hc

Calci ascorbat dihydrat; Mui calci ca acid 2,3-didehydroL-threo-hexono-1,4-lacton dehydrat.

M s C.A.S.

5743-27-1

Cng thc phn t

C12H14O12Ca.2H2O

Cng thc cu to

CH2OH
H C OH
O
Ca2+

O
H
-

OH

Khi lng phn t

426,35

3. Cm quan

Bt tinh th khng mi, mu trng hoc hi vng.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, rt t tan trong ethanol, khng tan trong

ether.

Calci

Phi c phn ng c trng ca calci.

Gc quay cc ring

Dung dch mu th trong nc nng 5% (kl/kl) c [ ]D25

trong khong +95 n +97o.

5.2. tinh khit

pH

6,0 - 7,5 (Dung dch 1/10).

Florid

Khng c qu 10,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C12H14O12Ca.2H2O

Khng thp hn 98,0% C12H14O12Ca.2H2O.

6. Phng php th
6.1. tinh khit

Florid

- Th theo JECFA monograph 1 - Vol. 4, phng php I.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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

Cn 0,4 g (chnh xc n mg) mu th cho vo bnh 250

ml, thm 50 ml nc khng c carbon dioxyd. Chun
ngay dung dch ny vi dung dch iod 0,1 N, khi gn t
im kt thc chun thm ch th l vi git dung dch h
tinh bt (TS) v chun tip n khi t im kt thc.
Mi ml dung dch iod 0,1 N tng ng vi 10,66 mg
C12H14O12Ca.2H2O.

Ph lc 4
YU CU K THUT V PHNG PHP TH I VI ASCORBYL PALMITAT
1. Tn khc, ch s

Vitamin C palmitate
INS 304
ADI = 1-1,25 mg/kg th trng

2. nh ngha
Tn ha hc

L-ascorbyl palmitat; Ascorbyl palmitat; Natri 2,3-didehydroL-threo-hexono-1,4-lacton-6-palmitat; 6-palmitoyl-3-keto-Lgulofuranolacton.

Cng thc phn t

C22H38O7

Cng thc cu to

O
CH2OC(CH2)14CH3
H C

OH
O
O

H
HO

OH

Khi lng phn t

414,55

3. Cm quan

Dng rn mu trng n trng vng, c mi ging qu h

cam, chanh.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Rt t tan trong nc, d tan trong ethanol.

Khong nng chy

107 oC 117 oC.

Phn ng kh

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 2,0%.

Gc quay cc ring

Dung dch mu th trong nc nng 10% (kl/tt) c [ ]D25

trong khong +21 v +24o.

Tro sulfat

Khng c qu 0,1%

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C22H38O7 Khng thp hn 95,0% tnh theo ch phm lm kh.

6. Phng php th
6.1. nh tnh
Phn ng kh

Dung dch mu th trong cn s lm mt mu ca dung

dch 2,6-diclorophenol indophenol (TS).

6.2. tinh khit

Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol. 4

- lm kh ti 56-60o trong chn khng, trong 1 gi.

Ch

- Th theo hng dn ti JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn 0,8 g (chnh xc n mg) cho vo hn hp gm 50 ml

nc khng c carbon dioxyd, 50 ml cloroform v 25 ml
dung dch acid sulfuric long (TS). Chun ngay dung
dch ny vi dung dch iod 0,1 N (ch cn lc u hn
hp), khi gn t im kt thc chun thm ch th l vi
git dung dch h tinh bt (TS) v chun tip n khi t
im kt thc.
Mi ml dung dch iod 0,1 N tng ng vi 20,73 mg
C22H38O7.

Ph lc 5
YU CU K THUT V PHNG PHP TH I VI ASCORBYL STEARAT
1. Tn khc, ch s

Vitamin C stearate
INS 305
ADI = 1 - 1,25 mg/kg th trng

2. nh ngha
Tn ha hc

L-ascorbyl stearat; Ascorbyl stearat; Natri 2,3-didehydro-Lthreo-hexono-1,4-lacton-6-stearat; 6-stearoyl-3-keto-Lgulofuranolacton.

Cng thc phn t

C24H42O7

M s C.A.S.

25395-66-8

Cng thc cu to

O
CH2OC(CH2)16CH3
H

OH
O
O

H
HO

OH

Khi lng phn t

442,6

3. Cm quan

Dng rn mu trng n trng vng, c mi ging qu h

cam, chanh

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan trong ethanol.

Khong nng chy

Khong 116 oC.

Phn ng kh

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 2,0%.

Tro sulfat

Khng c qu 0,1%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C24H42O7 Khng thp hn 95,0%.

6. Phng php th
6.1. nh tnh
Phn ng kh

Dung dch mu th trong cn s lm mt mu ca dung

dch thuc th 2,6-diclorophenol indophenol (TS).

6.2. tinh khit

Gim khi lng khi lm
kh

- Th theo hng dn ti JECFA monograph 1 - Vol. 4

- Lm kh ti 56-60o trong chn khng, trong 1 gi.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn 0,8 g (chnh xc n mg) cho vo hn hp gm 50 ml

nc khng c carbon dioxyd, 50 ml cloroform v 25 ml
dung dch acid sulfuric long (TS). Chun ngay dung
dch ny vi dung dch iod 0,1 N (ch cn lc u hn
hp), khi gn t im kt thc chun thm ch th l vi
git dung dch h tinh bt (TS) v chun tip n khi t
im kt thc.
Mi ml dung dch iod 0,1 N tng ng vi 22,13 mg
C24H42O7.

Ph lc 6
YU CU K THUT V PHNG PHP TH I VI ACID ERYTHORBIC
1. Tn khc, ch s

Acid erythorbic, Acid D-araboascorbic

INS 315
ADI khng gii hn

2. nh ngha
Tn ha hc

Acid D-erythro-hex-2-enoic deltalacton, Acid isoascorbic,

Acid D- isoascorbic

M s C.A.S.

89-65-9

Cng thc phn t

C6H8O6

Cng thc cu to

CH2OH
HO C H
O
O
H
HO

OH

Khi lng phn t

176,13

3. M t

Dng tinh th trng hoc hi vng, ng mu sm khi

ngoi nh sng.

4. Chc nng

Cht chng oxy ha

5. Tnh cht
5.1. nh tnh
tan

D tan trong nc, tan trong ethanol.

Khong nng chy

Khong 164 oC - 172oC, km theo phn hy.

Th ascorbat

Phi c phn ng c trng ca ascorbat.

Phn ng kh

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 0,4%.

Gc quay cc ring

[ ]D25 trong khong -16,5o v -18,0o.

Tro sulfat

Khng c qu 0,3%.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C6H8O6

Khng thp hn 99,0% tnh theo ch phm lm kh.

6. Phng php th
6.1. nh tnh
Phn ng kh

Dung dch mu th trong nc s kh ngay dung dch kali

permanganat (TS) m khng cn un nng, sn phm thu
c l kt ta mu nu.
Dung dch mu th trong cn s lm mt mu ca dung
dch 2,6-diclorophenol indophenol (TS).

6.2. tinh khit

Gim khi lng khi lm
kh

- Th theo JECFA monograph 1 - Vol. 4

- Lm kh di p sut gim, trn silicagel v trong 3 gi.

Tro sulfat

- Th theo JECFA monograph 1 - Vol.4, Phng php I.

- Cn 1g mu th.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn 0,4 g (chnh xc n mg) mu th c lm kh

trc, ha tan trong 100 ml nc khng c dioxyd carbon
v 25 ml dung dch acid sulfuric long (TS). Chun ngay
dung dch ny bng dung dch iod 0,1 N, khi gn t im
kt thc chun thm ch th l vi git dung dch h tinh
bt (TS) v chun tip n khi t im kt thc.
Mi ml dung dch iod 0,1N tng ng vi 8,806 mg
C6H8O6.

Ph lc 7
YU CU K THUT V PHNG PHP TH I VI dl--TOCOPHEROL
1. Tn khc, ch s

Vitamin E
INS 307c
ADI = 0,15 - 2 mg/kg th trng i vi dl-alpha-, & d-alphatocopherol, n cht hoc kt hp.

2. nh ngha
Tn ha hc

dl-5,7,8-Trimethyltocol, dl-2,5,7,8-tetramethyl-2-(4',8',12'trimethyltridecyl)-6-cromanol

M s C.A.S.

Khng s ng k C.A.S. Xc nh n l i vi ch phm

ny.
vitamin E: 59-02-9
alpha-tocopherol: 1406-18-4
all-rac-alpha-tocopherol: 2074-53-5
racemic-alpha-tocopherol c tng hp t phytol t nhin
hoc dn cht ca n: 10191-40-0.

Cng thc ha hc

C29H50O2

Cng thc cu to

CH3
H3C

CH3

CH3

CH3

CH3
CH3

HO
CH3

Khi lng phn t

430,71

3. Cm quan

Dng du snh, trong, gn nh khng mi, vng nht ti

h phch (Khi b oxy ha, en dn trong khng kh v
ngoi nh sng)

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan
Gc quay cc ring

Khng tan trong nc, d tan trong ethanol, ha ln c

vi ether.
20
D

: 00,05o (dung dch 1/10 trong cloroform)

Quang ph

Dung dch trong ethanol tuyt i c cc i hp th

khong 292 nm.

Phn ng mu

t yu cu (m t trong phn phng php th)

5.2. tinh khit

Ch s khc x

n (20, D): 1,503 - 1,507

Quang ph

E (1%, 1 cm) (292 nm): 71-76 (dung dch 0,01 g trong

200ml ethanol tuyt i).

Tro sulfat

Khng c qu 0,1%.

acid

t yu cu (m t trong phn phng php th).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng dl-alphatocopherol

Khng c nh hn 96,0% v khng c qu 102,0%.

6. Phng php th
6.1. nh tnh
Phn ng mu

Ha tan khong 0,01 g mu th trong 10 ml ethanol tuyt

i. Va thm 2 ml acid nitric va lc v un nng
khong 75 oC trong 15 pht. Xut hin mu ti ti mu
da cam.

6.2. tinh khit

Tro sulfat

- Th theo JECFA monograph 1 - Vol. 4, Phng php II

- Tin hnh th vi 1 g mu th.

acid

Ha tan 1 g mu th trong 25 ml hn hp ng th tch

ethanol v ether c trung tnh ha i vi
phenolphtalein (TS) bng natri hydroxyd 0,1 N, thm 0,5 ml
phenolphtalein (TS), v chun bng natri hydroxyd 0,1
N ti khi dung dch duy tr mu hng nht sau khi lc 30
giy. Lng dung dch natri hydroxyd 0,1 N tiu th khng
c nhiu hn 1,0 ml .

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- S dng k thut hp th nguyn t thch hp vi hm
lng quy nh xc 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.

6.3. nh lng

Phng php sc k kh lng

Thuc th v dung dch
Dung dch chun ni: Chun b dung dch trong n-hexan
cha 3 mg hexadecyl hexadecanoat, cn chnh xc, trong
mt ml.
Dung dch chun: ha tan khong 30 mg Alpha Tocopherol
chun i chiu USP hay tng ng, cn chnh xc,
trong 10,0 ml dung dch chun ni.
Dung dch th: ha tan khong 30 g mu th cn chnh
xc, trong 10,0 ml dung dch chun ni.
H thng sc k
Dng my sc k kh c detector ion ha ngn la v h
tim mu qua ng thy tinh hoc tim mu vo thng ct.

Trong iu kin in hnh, thit b gm ct thy tinh borosilicat 2-m 4-mm nhi diatomit 80-120 mesh cho sc k
silan ha, ra acid-base v tm 2% methylpolysiloxan.
Ct c duy tr ng nhit trong khong 240oC v 260oC,
bung tim khong 290oC, v detector khong 300oC. iu
chnh tc kh mang kh thu c pic hexadecyl
hexadecanoat khong 18 ti 20 pht sau khi bm mu
khi dng ct 2%, hoc 30 ti 32 pht khi dng ct 5%.
(CH : X l v luyn ct nu cn).
Tnh ph hp ca h thng
Chy sc k mt s va mu tim hn hp trong nhexan ca 1 mg/ml mi cht Alpha Tocopherol chun i
chiu v Alpha Tocopheryl Acetat chun i chiu, nh ch
dn trong phn chun ha, m bo rng phn gii,
R, khng c nh hn 1,0.
Chun ha
Chy sc k lin tip nhng lng 2- ti 5-L dung dch
chun ti khi h s p ng tng i F khng i (tc l,
thay i trong khong 2%) i vi ba ln tim lp li lin
tip. Nu dng tch phn, iu chnh thit b thu c t
nht pic hexadecyl hexadecanoat nm trong khong ti a
l 70% thang ghi. o din tch cc pic chnh xut hin ti
thi gian lu tng i khong 0,51 (alpha-tocopherol) v
1,00 (hexadecyl hexadecanoat), v ghi gi tr ln lt l Ac
v A1. Tnh h s p ng tng i, F, theo cng thc:
(Ac/A1) (C1/CC)
Trong :
C1 v Cc ln lt l nng chnh xc, tnh bng mg/ml,
ca hexadecyl hexadecanoat v Alpha Tocopherol chun
i chiu USP trong dung dch chun.
Tin hnh
Bm mt th tch thch hp (2 ti 5 L) dung dch th vo
h thng sc k, v ghi sc . Ghi din tch pic chnh xut
hin ti thi gian lu tng i khong 0,51 (alphatocopherol) v 1,00 (hexadecyl hexadecanoat), v ghi gi tr
ln lt l at v a1.
Tnh khi lng, mg, ca dl-alpha-tocopherol trong mu
th theo cng thc:
(10C1/F) (at/a1).

Ph lc 8
YU CU K THUT V PHNG PHP TH I VI PROPYL GALAT
1. Tn khc, ch s

INS 310
ADI = 0 1,4 mg/kg th trng

2. nh ngha
Tn ha hc

Propyl galat, ester propyl ca acid gallic, ester n-propyl ca

acid 3,4,5-trihydroxybenzoic, propyl 3,4,5-trihydroxybenzoat

M s C.A.S.

121-79-9

Cng thc ha hc

C10H12O5

Cng thc cu to

HO

CH3

OH
OH

Khi lng phn t

212,20

3. Cm quan

Cht rn kt tinh khng mi, mu trng hoc trng ng.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Tan t trong nc, d tan trong ethanol, ether v propan1,2-diol.

Khong nng chy

146 150 oC sau khi lm kh.

Acid galic

t yu cu (m t trong phn phng php th).

Sc k lp mng-tch cc t yu cu (m t trong phn phng php th).

ester galat
5.2. tinh khit
Mt khi lng khi lm Khng c qu 0,5%.
kh
Tro sulfat

Khng c qu 0,1%

Hp cht hu c Clor ha Khng c qu 100,0 mg/kg tnh theo clor.

Acid t do

Khng c qu 0,5% tnh theo acid galic.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng C10H12O5 Khng c nh hn 98,0% v khng ln hn 102,0% tnh

theo ch phm kh.
6. Phng php th
6.1. nh tnh
Acid galic

Ha tan khong 0,5 g mu th trong 10 ml dung dch natri

hydroxyd (TS) v un si trong 30 pht di lung kh nit.
Duy tr dng kh nit, lm ngui hn hp v acid ha ti pH
2-3 bng acid sulfuric (TS). Lc ta qua phu lc thy tinh
xp, ra bng mt lng ti thiu nc v sau lm kh
110 C trong 2 gi. im chy ca acid galic thu c
khong 240 C, km phn hy.

Sc k lp mng-tch cc Dng bn mng trng silica gel G. Chun b dung dch th

bng cch ha tan 10 mg mu th trong 10 ml ethanol.
ester galat
Chun b dung dch i chng A bng cch ha tan 10 mg
propyl galat trong 10 ml ethanol v dung dch i chng B
bng cch ha tan 10 mg propyl galat v 10 mg octyl galat
trong 10 ml ethanol.
Chm 5 L mi dung dch ln bn mng. Trin khai sc k
khong 15 cm k t im xut pht dng dung mi trin
khai gm acid acetic bng, ether du ha v toluen (1:2:2).
kh bn mng ngoi khng kh. Phun ln bn mng
dung dch ch th acid phosphomolybdic 20% (kl/tt) trong
ethanol ti khi nhum mu vng bn.
Kim tra di nh sng thng. Sau vi pht, c s
chuyn mu dn thnh mu xanh l. Sau 5 ti 10 pht
bn mng thm hi amoniac ti khi nn c mu trng.
Kim tra di nh sng thng. Vt chnh ca dung dch
th tng ng vi vt propyl galat ca cc dung dch i
chng. phn gii thch hp gia vt ca propyl v octyl
galat c xc nh da vo dung dch i chng B.
6.2. tinh khit
Mt khi lng khi lm - Th theo JECFA monograph 1 - Vol. 4
- sy ti 110 C trong 4 gi.
kh
Ch : Nn cho thng gi trong qu trnh sy.
Tro sulfat

- Th theo JECFA monograph 1 - Vol. 4, Phng php I

- Cn 2 g mu th.

Hp cht hu c Clor ha Ha tan 1 g mu th trong 10 ml natri hydroxyd 0,1 N. Acid

ha bng acid nitric (TS) v lc ly ta. Trn ta vi 2 g
calci carbonat, lm kh hn hp v nung. Ha tan cn
trong 20 ml acid nitric long (TS) v lc. Trn dung dch ny
vi 0,5 ml bc nitrat 0,1 N. c ca dung dch ny phi
khng c hn c thu c ca 20 ml acid nitric long
(TS) cha 0,5 ml bc nitrat 0,1 N v 0,3 ml acid hydrocloric
0,01 N.

Acid t do

Thm 5 git xanh lc bromocresol (TS) vo hn hp gm

50 ml nc khng c carbon dioxyd v 50 ml aceton,
chun bng acid hydrocloric 0,005 N ti khi mu ca
dung dch ging nh mu ca m (pH 5) (TS) c cng
lng cht ch th. Ha tan 0,4 g mu th trong 50 ml
aceton v thm 50 ml nc khng c carbon dioxyd, 5 git
xanh lc bromocresol (TS) v mt lng acid hydrocloric
0,005 N nh dng trong php th trc a dung
mi v pH 5. Chun dung dch ny ti pH 5 bng natri
hydroxyd 0,05 N, i chiu vi m (pH 5) (TS).
Mi ml natri hydroxyd 0,05 N tng ng vi 8,506 mg acid
galic.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- S dng k thut hp th nguyn t thch hp cho hm
lng quy nh xc 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.

6.3. nh lng

Cn chnh xc khong 0,2 g mu th sy kh vo cc

400 ml. Thm 150 ml nc v un nng ti si. Sau ,
va khuy mnh lin tc, va thm 50 ml bismuth (II) nitrat
(TS). Tip tc khuy trong vi pht ti khi ta hon ton,
sau dung dch ngui ti nhit phng. Lc ta vng
qua phu lc thy tinh xp cn b, u tin ra vi acid
nitric 0,05 N lnh v sau bng nc , ti khi ht acid.
Sy 110 oC ti khi lng khng i. Tin hnh nh ch
dn trong tiu chun i vi dodecyl galat. Tnh hm lng
propyl galat theo cng thc:
Khi lng kt ta 48,63
% Propyl galat = ---------------------------------------Khi lng mu th

Ph lc 9
YU CU K THUT V PHNG PHP TH I VI NHA GAIAC
1. Tn khc, ch s

Gm Guaiac, Gum Guaiac, Gum Guaiacum, Guaiacum

INS 314
ADI = 0 - 2,5 mg/kg th trng

2. nh ngha

L nha t g cy Guajacum officinale L., hoc cy

Guajacum sanctum L., (Fam. Zygophyllaceae), cha khong
70% acid alpha- v beta-guaiaconic, 10% acid guaiaretic v
15% nha guaiac beta v lng nh guaiac vng, vanilin...

3. Cm quan

Dng cc kch thc khng u, km theo cc mnh m

thc vt hoc dng khi ln hnh trn hoc hnh trng, bn
ngoi c mu nu en hoc nu sm, khi ra ngoi lu c
mu xanh lc, b mt khi khi nt to thnh khe nh thy
tinh bng, dng ming mng th trong sut v c mu t nu
n vng nu, chuyn thnh mu nu olive khi ngoi
khng kh. C mi thm nh.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, tan trong cht bo, d tan nhng tan
khng hon ton trong ethanol, ether v dung dch kim.

Khong nng chy

85 90 oC.

Phn ng mu

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Tro ton phn

Khng c qu 5,0%.

Tro khng tan trong acid Khng c qu 2,0%.

Cn khng tan trong
ethanol

Khng c qu 15,0%.

Rosin

t yu cu (m t trong phn phng php th).

Ch

Khng c qu 2,0 mg/kg.

6. Phng php th
6.1. nh tnh
Phn ng mu

Thm 1 git dung dch st (III) clorid (TS) vo 5 ml dung dch

mu th trong ethanol (1/100). Dung dch c mu xanh lam
V dn chuyn thnh mu xanh lc cui cng chuyn thnh
mu vng xanh.
Hn hp gm 5 ml dung dch mu th trong ethanol (1/100)

v 5 ml nc s chuyn thnh mu xanh lam khi lc vi 20

mg ch peroxyd. Lc dung dch v chia i dch lc. Mt phn
em un si, dung dch s mt mu nhng nu lc vi ch
peroxyd th mu li xut hin. Thm vi git dung dch acid
hydrocloric long (TS) vo phn dch lc cn li, dch lc s
mt mu ngay.
6.2. tinh khit
Cn khng tan trong
ethanol

Cn 2 g (chnh xc n mg) mu th c nghin mn

cho vo mt ng lt kh, cn b (chuyn dng chit),
tin hnh chit bng thit b chit lin tc vi dung mi
ethanol trong 3 gi n khi chit c hon ton. Sy
kh phn cn cn li trong ng lt ti 105 oC trong 4 gi,
cn. Khi lng cn cn li khng c qu 300 mg.

Rosin

Dung dch mu th 10% trong ether du ha khng c mu.

Khi lc dung dch ny vi ng lng dung dch ng (II)
acetat 0,5%, hn hp c mu xanh lc, nhng mu khng
c m hn mu ca hn hp gm dung dch ng (II)
acetat tng t trong ether du ha.

Ch

- Th theo hng dn ti JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut hp th nguyn t thch hp cho
hm lng quy nh. La chn c mu th v phng php
chun b mu da trn nguyn tc ca phng php m t
trong JECFA monograph 1 - Vol. 4 - phn cc phng php
phn tch cng c.

Ph lc 10
YU CU K THUT V PHNG PHP TH I VI
tert-BUTYLHYDROQUINON
1. Tn khc, ch s

Tertiary butylhydroquinone; TBHQ

INS 319
ADI = 0 - 0,7 mg/kg th trng

2. nh ngha
Tn ha hc

Mono-tert-butylhydroquinon; t-butylhydroquinon; 2-(1,1dimethylethyl)-1,4-benzendiol

M s C.A.S.

1948-33-0

Cng thc ha hc

C10H14O2

Cng thc cu to

OH

CH3
C CH
3
CH3

OH
Khi lng phn t

166,22

3. M t

Tinh th mu trng c mi c trng nh.

4. Chc nng

Cht chng oxy ha

5. Tnh cht
5.1. nh tnh
tan

Thc t khng tan trong nc, tan trong ehanol.

im nng chy

Khng thp hn 126,5oC.

Cc phenol

t yu cu (m t trong phn phng php th).

5.2. tinh khit

t-Butyl-p-benzoquinon

Khng c qu 0,2%.

2,5-Dibutyl-hydroquinon

Khng c qu 0,2%.

Hydroquinon

Khng c qu 0,1%.

Toluen

Khng c qu 25,0 mg/kg.

Ch

Khng c qu 2,0 mg/kg.

5.3.
Hm
C10H14O2

lng Khng thp hn 99,0% C10H14O2.

6. Phng php th
6.1. nh tnh
Cc phenol

Ha tan 5 mg mu th trong 10 ml methanol, thm 10,5 ml

dung dch dimethylamin (1/4). Hn hp c mu n hng.

6.2. tinh khit

t-Butyl-p-benzoquinon

Thit b:
S dng my quang ph hng ngoi hai chm tia. Cuvet c
ca s CaF2 vi chiu dy lp mu lng l 0,4 mm.
Thuc th v cc dung dch:
Chun b dung dch chun: Cn chnh xc 10 mg mono -tertbutyl-p-benzoquinon chun tham chiu USP v chuyn vo
trong bnh nh mc 10 ml, ho tan trong cloroform, pha
long v nh mc n 10 ml bng dung mi trn ri trn
u.
Chun b mu th: Cn chnh xc 1 g mu c nghin
thnh bt mn trong my nghin cao tc ri cho vo bnh
nh mc 10 ml, ho tan trong cloroform, pha long n
10 ml bng dung mi trn ri trn u. Lc dung dch qua
mng lc Millipore (UHWPO 1300) hoc tng ng trc
khi tin hnh th.
Tin hnh:
Cho cloroform vo cuvet so snh v cho dung dch chun
vo cuvet o mu th. t ln lt cc cuvet ny vo v tr
o ca my. Ghi li ph hng ngoi t s sng 1600 n
1775cm-1. Trn ph, v ng nn t 1612 n 1750cm-1 v
xc nh hp th ( tr nn) AS ca dung dch chun ti
s sng 1659cm-1, xc nh hp th AU ca dung dch
mu ti s sng 1659cm-1.
Tnh kt qu: Tnh hm lng (%) ca t-butyl-p-benzoquinon
trong mu th theo cng thc:
(%) = 100 AU/AS WS / W U
Trong :
WS: khi lng chnh xc ca mono tert-butyl-p benzoquinon
chun (mg).
WU: khi lng chnh xc ca mu th (mg)

Hydroquinon v 2,5- Thit b:

dibutyl-hydroquinon
My sc k kh thch hp ghp ni vi detertor dn nhit
(loi 810 F, M hoc tng ng) gm ct thp khng g c
kch thc 0,61 m (2ft) x 6,35 mm (ng knh ngoi). Cht
nhi ct gm 20% silicon SE-30 v 80% l diatoport S (60/80
mesh) hoc cc vt liu tng ng.
iu kin vn hnh:
Cc thng s vn hnh c th bin i tu thuc vo tng
thit b. Tuy nhin c th s dng cc iu kin sau thu
c sc k ph hp:

Nhit ct: lp chng trnh t 100 oC n 270 oC, vi tc

gia nhit 15 oC/1 pht
Nhit bung bm mu: 300 oC
Kh mang: He, tc dng l 100 ml/pht
Dng cu o: 140 mA
nhy: 1x i vi tch phn k (Infotronics CRS-100), 2x
cho my ghi
Thuc th v cc dung dch:
Dung dch gc: cn chnh xc 50 mg hydroquinon (HQ), 50
mg 2,5-di-t-butylhydroquinon (DTBHQ) v 50 mg methyl
benzoat (cht ni chun) ri chuyn vo 3 bnh nh mc 50
ml ring bit, pha long n 50 ml bng pyridin v trn
u.
Dy dung dch chun: Ly 0,5 ml; 1 ml; 2 ml v 3 ml dung
dch gc HQ vo 4 bnh nh mc 10 ml ring bit, cho thm
2 ml dung dch methyl benzoat (cht ni chun) vo mi
bnh, pha long cho 10 ml bng pyridin ri trn u.
Tng t, pha 4 dung dch chun DTBHQ. Chun b dn
xut trimethylsilyl cho mi dung dch nh sau: ly 9 git dung
dch chun vo syring kh 2 ml, thm 250 L N,Obistrimethylsilylacetamid, un nng 80oC trong 10 pht.
Chy sc k hai ln, mi ln 10 l ca mi dung dch chun
v v th biu th tng quan gia t l nng ca HQ
trn nng cht ni chun (trc X) vi t l p ng ca
HQ trn p ng ca cht ni chun (trc Y). Tng t, v
th biu th tng quan gia DTBHQ v cht ni chun.
Tin hnh th:
Cn khong 1 g (chnh xc n mg) mu ri chuyn vo
bnh nh mc 10 ml, cho thm 2 ml dung dch ni chun gc
methyl benzoat, pha long ti 10 ml bng pyridin ri trn
u. Chun b dn xut trimethylsilyl ging nh trong phn
chun b dy dung dch chun trn. Sau chy sc k hai
ln, bm 10 L mi ln ghi sc k . Thi gian lu gn
ng ca cc pic: methyl benzoat: 2,5 pht; dn xut TMS
ca HQ: 5,5 pht; dn xut TMS ca TBHQ: 7,3 pht; dn
xut TMS ca DTBHQ: 8,4 pht.
Tnh kt qu:
Xc nh din tch pic (p ng). Tnh t s p ng ca HQ
v DTBHQ so vi cht ni chun.
T ng chun, xc nh t l nng ca HQ v DTBHQ
trn cht ni chun v tnh % ca HQ v % DTBHQ trong
mu theo cng thc:
A = Y I 10/S
Trong : A l hm lng (%) HQ hoc DTBHQ trong mu.
Y l t l nng (trc X trn ng chun).
I l % (kl/tt) ca cht ni chun trong dung dch mu th
S l khi lng ca mu th (g).

Toluen

Thit b:
My sc k kh ghp ni vi detector ion ho ngn la (loi
F, M 810 hoc tng ng) gm ct thp khng g c kch
thc 3,66 m x 3,18 mm (ng knh ngoi). Pha tnh l
10% (theo khi lng) sillicon SE-30 v 90% diatoport S
(60/80 mesh) hoc cc vt liu tng ng.
iu kin vn hnh
Cc thng s vn hnh c th bin i tu thuc vo tng
thit b. Tuy nhin c th s dng cc iu kin sau thu
c sc k ph hp:
Nhit ct: chng trnh nhit t 70 oC n 280 oC vi tc
gia nhit l 15 oC /pht v gi yn.
Nhit bung bm mu: 275 oC
Nhit cell: 300 oC
t H2 v O2 (hoc khng kh) : 1,4 atm (20 Psi) cho mi kh
Thuc th v cc dung dch:
Dung dch chun: Chun b dung dch toluen trong octanol
cha khong 50 g/ ml. Tnh nng thc (Cr) (%, kl/tt)
Dung dch mu: Cn chnh xc 2 g mu ri chuyn vo trong
bnh nh mc 10 ml, ho tan trong octanol, pha long cho
10 ml bng dung mi trn v trn u. Tnh nng thc
ca dung dch (Cs) (%, kl/tt)
Tin hnh:
Bm 5 l dung dch chun vo trong my sc k v o chiu
cao pic toluen (Hr) trn sc . Thi gian lu ca toluen l
3,3 pht. Nhng pic khc l khng cn quan tm n trong
php phn tch ny.
Tng t, bm 5 l dung dch mu v 5 l mu trng
octanol vo my sc k ri o chiu cao pic ca toluen (Hs)
Tnh kt qu:
Hm lng toluen trong mu th (mg/kg) c tnh theo
cng thc sau
HS/HR CR/CS 106

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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).

6.3. nh lng

Cn chnh xc 170 mg mu nghin thnh bt mn, chuyn

vo bnh nn ming rng 250 ml, ho tan trong 10 ml
ethanol. Cho thm 150 ml nc ct, 1 ml H2SO4 1 N v 4
git ch th diphenylamin (3 mg Natri p-diphenylamin sulfonat
trong 1 ml H2SO4 0,1 N). Chun bng ceri sulfat 0,1N ti
khi mu dung dch chuyn t mu vng sang tm . Ghi li

th tch (ml) ca ceri sulfat 0,1 N (V) dng.

Tnh hm lng (%) ca C10H14O2 trong mu, khng hiu
chnh i vi hydroquinon (HQ) v 2,5 di-tert-butylhydroquinon (DTBHQ) theo cng thc sau:
(V 0,1 ml) N 8,311/W
Trong :
0,1 ml : th tch ca ceri sulfat tiu hao do cc sn phm oxy
ho s cp ca tert - butylhydroquinon c trong mu.
N : nng thc ca dung dch ceri sulfat
W : khi lng ca mu (g).
Ghi li % cha hiu chnh tnh c nh trn l A. Nu HQ
v DTBHQ c mt trong mu, chng cng tham gia vo qu
trnh chun .
Tnh hm lng c hiu chnh (%) ca C10H14O2 trong
mu theo cng thc sau:
A - (%HQ 1,51) - (%DTBHQ 0,75)
S dng gi tr % HQ v %DTBHQ xc nh c bng
phng php sc k kh trn.

Ph lc 11
YU CU K THUT V PHNG PHP TH I VI BUTYLHYDROXYANISOL
1. Tn khc, ch s

Butylated hydroxyanisole; BHA

INS 320
ADI = 0 - 0,5 mg/kg th trng

2. nh ngha
Tn ha hc

3-Tert-butyl-4-hydroxyanisol; hn hp ca 3- v 2-tert-butyl4-hydroxyanisol

M s C.A.S.

25013-16-5

Cng thc ha hc

C11H16O2

Cng thc cu to

OH

OH

C(CH3)3

C(CH3)3
OCH3

Khi lng phn t

ng phn v tr 3
180,25

OCH3

ng phn v tr 2

3. Cm quan

Cht rn dng sp hoc tinh th mu trng hoc vng nht,

c mi c trng nh.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, d tan trong propan-1,2-diol v

ethanol.

Phn ng mu

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Tro sulfat

Khng c qu 0,05%.

Ch

Khng c qu 2,0 mg/kg.

Tp cht phenol

Khng c qu 0,5%.

5.3.
Hm
C11H16O2

lng Khng thp hn 98,5% C11H16O2 v khng thp hn 85% 3tert-butyl-4-hydroxyanisol.

6. Phng php th
6.1. nh tnh

Phn ng mu

Ly 5 ml dung dch mu th 1/10.000 trong ethanol 72%,

thm 2 ml dung dch natri borat (TS) v 1 ml dung dch 2,6dicloroquinonclorimid 1/10.000 trong ethanol tuyt i, lc
u. xut hin mu xanh lam.

6.2. tinh khit

Tro sulfat

- Th theo JECFA monograph 1 - Vol. 4, Phng php I.

- Cn 5 g mu.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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.

Tp cht phenol

- Xc nh bng sc k lp mng: dng bn mng silicagel

G.
Dung dch 1: Ho tan 0,25 g mu th trong 10 ml ether
Dung dch 2: Pha long 1 ml dung dch 1 ti 10 ml bng
ether v tip theo pha long 1 ml dung dch ny ti 20 ml
bng ether. S dng dung dch pha long cui cng l dung
dch 2.
- Tin hnh

6.3. nh lng

Ln lt chm 2 L dung dch 1 v dung dch 2 trn cc bn

sc k ring bit. t bn mng vo trong bnh sc k
bo ha dung mi cloroform. dung mi khai trin cch
vch xut pht 15 cm. Ly bn mng ra khi bnh sc k,
phun ln bn mng hn hp gm dung dch st (III) clorid
2% v kali fericyanid 1% mi pha. Trn bn mng xut hin
cc vt mu xanh, cc vt ny s hin r hn bng cch
phun acid hydrocloric 2 N ln bn mng.
Bt k vt mu xanh no xut hin trn Sc k ca dung
dch 1 (ngoi vt chnh v vt c Rf = 0,35) khng c m
hn so vi vt chnh xut hin trong sc k ca dung dch
2.
Phng php sc k kh
Dung dch ni chun (c th tu chn Diphenylamin hoc 4tert-butylphenol). Cn chnh xc 500 mg cht ni chun ho
tan v nh mc ti 250 ml bng aceton.
Dung dch chun:
Cn chnh xc 90 mg 3-butyl hydroxyanisol v 10 mg 2-butyl
hydroxyanisol, ho tan v nh mc n 100 ml trong dung
dch ni chun.
Tin hnh:
Cn chnh xc 10 mg mu th, ho tan v nh mc n 50
ml bng dung dch ni chun. Bm nhiu ln dung dch ny
vo thit b sc k kh vi detetor ion ho ngn la. iu
kin lm vic nh sau:

A: iu kin cht ni chun ra gii ra sau 3-tert-butyl-4hydroxyanisol:

Ct: Ct thu tinh kch thc 1,5 m x 2 mm
Cht nhi: 10% XE-60 c ht 100 200 mesh
Nhit ct: 155 oC
Nhit detector: 250 oC
Nhit bung bm mu: 250 oC
Kh mang: Nit, tc dng 30 ml/pht
B: iu kin cht ni chun ra gii ra trc 3-ter-butyl4-hydroxyanisol:
Ct: Ct thu tinh kch thc 2 m x 3 mm
Cht nhi: 5% Versamit-900 c ht 80/100 mesh cromosorb
W-AW- DMCS
Nhit ct: 170 oC
Nhit bung bm: 225 oC
Nhit detector: 250 oC
Kh mang: Nit, tc dng 30 ml/pht.
Dng ng chun biu th tng quan gia chiu cao pic
2- v 3-butyl hydroxyanisol vi nng chun.
Bm dung dch mu. Da vo ng chun xc nh nng
2- v 3- butyl hydroxy anisol. Tng hm lng ng phn
2- v 3- chnh l hm lng ca mu th.
C th s dng phng php sc k kh khc nh sau:
Chun b mu th: cn chnh xc khong 100 mg mu ho
tan v pha long ti 10 ml vi dung dch chun ni.
H thng sc k: H thng sc k kh c ct bng thp
khng g kch thc 1,8 m x 2 mm, c nhi cht mang
tm 10% pha tnh lng, ct c luyn trong ch ng
nhit nhit trong khong 175 n 185 oC; ghp ni vi
detector ion ho ngn la, kh mang s dng l heli. Bm
dung dch chun vo my, s lng dng ng
chun m bo chc chn rng lch chun tng i
khng vt qu 2% vi ng phn 3-tert-butyl-4hydroxyanisol v khng vt qu 6% vi ng phn 2-tertbutyl-4-hydroxyanisol, ghi li pic. H s phn gii gia cc
ng phn khng c thp hn 1,3 v h s dong pic
khng c vt qu 2.
Pha tnh lng: 25% 2-cyanoethyl v 75% methyl-polysiloxan
Cht mang: t silic dng cho sc k c nung chy bng
cch trn hn hp diatomit vi Na2CO3 nung chy v nung
900 oC. t silic c ra bng acid, sau c ra bng
nc cho n khi trung tnh nhng khng c ra bng
kim. t silic c silan ha bng cch x l vi tc nhn
nh dimethyldiclorosil che ph cho b mt nhm silanol.
Tin hnh:
Bm ln lt (khong 5 l) dung dch chun v dung dch

chun b th vo my sc k kh, ghi li sc k . o din

tch pic ca mi ng phn v chun ni trong mi sc .
Tnh kt qu:
Khi lng (mg) ca mi ng phn trong mu th c
tnh theo cng thc: 10 CS (RU/RS)
Trong
Cs: nng ca ng phn trong dung dch chun (mg),
Rs: t s din tch pic ca mi ng phn so vi cht ni
chun trn cng sc k chun.
RU : t s din tch ca mi ng phn so vi cht ni chun
trn cng sc k mu th.
Tnh khi lng (mg) ca C11H16O2 trong mu th bng cch
ly tng khi lng ca 2 ng phn.

Ph lc 12
YU CU K THUT V PHNG PHP TH I VI BUTYLHYDROTOLUEN
1. Tn khc, ch s

BHT
INS 321
ADI = 0 - 0,3 mg/kg th trng

2. nh ngha
Tn ha hc

2,6-Ditertiary-butyl-p-cresol; 4-methyl-2,6-ditertiary-butylphenol

M s C.A.S.

128-37-0

Cng thc ha hc

C15H24O

Cng thc cu to

OH
(CH3)3C

C(CH3)3

OCH3

Khi lng phn t

220,36

3. Cm quan

Cht rn dng vy hoc tinh th mu trng, khng mi hoc

c mi thm nh c trng.

4. Chc nng

Cht chng oxy ha

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v propan-1,2-diol, d tan trong

ethanol.

Khong nng chy

69,0o 72,0oC

Quang ph

t yu cu (m t trong phn phng php th).

Phn ng mu

t yu cu (m t trong phn phng php th).

5.2. tinh khit

Nhit ng c

Khng c thp hn 69,2 oC.

Tro sulfat

Khng c qu 0,005%.

Ch

Khng c qu 2,0 mg/kg.

Tp cht phenol

Khng c qu 0,5%.
Xem hng dn trong phn phng php th

5.3. Hm lng C15H24O Khng thp hn 99,0%.

6. Phng php th
6.1. nh tnh
Quang ph

o hp th ca lp dy 2 cm dung dch mu th
1/100.000 trong ethanol loi nc trong vng bc sng
t 230 nm n 320 nm, ch cho duy nht 1 cc i hp th
ti 278 nm.

Phn ng mu

Ly 10 ml dung dch mu th 1/100.000 trong methanol,

thm 10 ml nc ct, 2 ml dung dch NaNO2 (3/1000) v 5
ml dung dch dianisidin dihydroclorid (Cn 200 mg 3,3dimethoxy-benzidin dihydroclorid ho tan trong hn hp gm
40 ml dung dch methanol v 60 ml acid hydrocloric 1N).
Trong 3 pht dung dch s xut hin mu cam. Thm 5 ml
cloroform v lc u. Lp cloroform xut hin mu tm hoc
hi ta, mu ny b phai dn khi a ra nh sng.

6.2. tinh khit

Tro sulfat

- Th theo JECFA monograph 1 - Vol. 4, Phng php I.

- Cn 20 g mu.

Ch

- Th theo JECFA monograph 1 - Vol. 4.

- Xc nh bng k thut 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.

Tp cht phenol

Xc nh bng sc k lp mng: dng bn mng silicagel G.

Dung dch 1: Ho tan 0,25 g mu th trong 10 ml ether
Dung dch 2: Pha long 1 ml dung dch 1 ti 10 ml bng
ether v tip theo pha long 1 ml dung dch ny ti 20 ml
bng ether. S dng dung dch pha long cui cng l dung
dch 2.
Tin hnh

6.3. nh lng

Ln lt chm 2 L dung dch 1 v dung dch 2 trn cc bn

sc k ring bit. t bn mng vo trong bnh sc k
bo ha dung mi cloroform. dung mi khai trin cch
vch xut pht 15 cm. Ly bn mng ra khi bnh sc k,
phun ln bn mng hm hp gm dung dch st (III) clorid
2% v kali fericyanid 1% mi pha. Trn bn mng xut hin
cc vt mu xanh, cc vt ny s hin r hn bng cch
phun acid hydrocloric 2 N ln bn mng.
Bt k vt mu xanh xut hin trn Sc k ca dung dch
1 (ngoi vt chnh v vt) khng c m hn so vi vt
chnh xut hin trong sc k ca dung dch 2.
Phng php sc k kh (JECFA monograph 1 - Vol. 4)
Dung dch ni chun: (cht ni chun tu chn diphenylamin
hoc 4-tert-butylphenol). Cn chnh xc 500 mg, ho tan
trong aceton v dng aceton nh mc n 250 ml.

Dung dch chun: Cn chnh xc 100 mg butyl hydroxytoluen

ho tan trong aceton v dng aceton nh mc n 50 ml.
Tin hnh:
Cn chnh xc 10 mg mu th, ho tan vo dung dch ni
chun v nh mc n 50 ml. Bm dung dch ny vo
my sc k kh vi iu kin sau:
Ct thu tinh kch thc 1,5 m x 3 mm nhi 10% XE-60 trn
100 - 2000 mesh, hoc tng ng;
Nhit ca bung bm mu v ca detector tng ng l
225 oC v 250 oC. Nhit ct l 155 oC.
Kh mang l nit vi tc 30 ml/pht
Detector ion ho ngn la (FID)
Dng th chun biu din t s chiu cao pic bytyl
hydroxytoluen/chiu cao pic ni chun ti cc nng xc
nh khc nhau. Nng ca butyl hydroxytoluen c xc
nh bng ni suy t th chun.

Ph lc 12
YU CU K THUT V PHNG PHP TH
I VI DILAURRYL THIODIPROPIONAT
1. Tn khc, ch s

Dilauryl thiodipropionate
INS 389
ADI = 0 - 3 mg/kg th trng

2. nh ngha

Ester ca acid thiodipropionic v lauryl alcohol thc phm

Tn ha hc
Ch s C.A.S.

Didodecyl 3,3'-thiodipropionic; Ester Dilauryl ca acid , 'thiodipropionic

123-28-4

Cng thc phn t

C30H58O4S

Cng thc cu to

CH2

CH2

COO(CH2)11CH3

CH2

COO(CH2)11cH3

S
CH2
Khi lng phn t

514,86

3. M t

Tinh th dng vy mu trng, c mi c trng ging

ester ngt.

4. Chc nng

Cht chng oxy ha.

5. Tnh cht
5.1. nh tnh
tan

Khng tan trong nc, tan trong ethanol v ete.

im ng c

Khng thp hn 40o.

Ch s x phng ha

205,0 215,0.

5.2. tinh khit

Acid

Khng c qu 0,2% (tnh theo acid thiodipropionic).

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng
C30H58O4S

Khng thp hn 99,0%.

6. Phng php th
6.1. tinh khit
Tnh acid

Thm 5 git dung dch phenolphtalein (TS) v 50 ml hn

hp gm 1 phn methanol v 3 phn benzen, trung ha
hn hp bng dung dch kali hydroxyd trong ethanol. Cn
2 g (chnh xc n mg) mu th, cho vo hn hp

chun b trn, khuy u cho tan hon ton v chun

vi dung dch kali hydroxyd trong ethanol 0,1 N.
Mi ml dung dch kali hydroxyd trong ethanol 0,1 N tng
ng vi 8,91 mg C6H10SO4.
Ch

- Th theo monograph 1 - Vol.4.

- Xc nh bng k thut 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

Cn 700 mg (chnh xc n mg) mu th, cho v bnh

nn 250 ml, thm 100 ml acid acetic v 50 ml ethanol,
un nng nh hn hp n khi mu th tan hon ton.
Thm 3 ml acid hydrocloric v 4 git dung dch pethoxychrysoidin (TS) v chun ngay vi dung dch
bromid-bromat 0,1 N (TS). Khi gn n im tng
ng (dung dch c mu hng) thm tip 4 git ch th v
tip tc chun chm (tng git), n khi dung dch
chuyn t mu sang mu vng nht. Tin hnh lm
mu trng song song v hiu chnh kt qu nu cn.
Mi ml dung dch bromid-bromat 0,1 N (TS) tng ng
vi 25,74 mg C30H58SO4. Tnh hm lng % v tr i
hm lng acid dithiopropionic (kt qu phn th acid)
thu c kt qu hm lng C30H58SO4.