QCVN4 6 ChatChongOxiHoa

CNG HO 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 tert-butylhydroquinon.
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-threo-hexono-1,4lacton; 3-keto-L-gulouranolacton
M s C.A.S.
50-81-7
Cng thc phn t
C6H8O6
Cng thc cu to
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
5.2. tinh khit

Gim khi lng khi lm kh
Khng c qu 0,4%.
Gc quay cc ring
[]D25 trong khong +20,5 v +21,5o.
pH
2,4 2,8 (Dung dch 1/50).
Tro sulfat
Khng c qu 0,1%.
Ch
Khng c qu 2 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 2,6diclorophenol indophenol (TS).
5.2. tinh khit
- 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 C 6H8O6.
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-L-threo-hexono-1,4lacton enolat; Natri 3-keto-L-gulofuranolacton enolat.
M s C.A.S.
134-03-2
Cng thc phn t
C6H7O6Na
Cng thc cu to
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
5.2. tinh khit

Khng c qu 0,25%.
Gc quay cc ring
Dung dch mu th trong nc nng 10% (kl/tt) c []D25 trong khong

+103 v +108o.
pH
6,5 - 8,0 (Dung dch 1/10).
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng C6H7O6Na
6. Phng php th
6.1. nh tnh
Natri

- 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 2,6-diclorophenol

indophenol (TS).
6.2. tinh khit


- Lm kh:trn acid sulfuric trong bnh chn khng, trong 24 gi.
Ch
- Th theo JECFA monograph 1 - Vol. 4.

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 C 6H7O6Na.
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-didehydro-L-threohexono-1,4-lacton dehydrat.
M s C.A.S.
5743-27-1
Cng thc phn t
C12H14O12Ca.2H2O
Cng thc cu to
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 mg/kg.
Ch
Khng c qu 2mg/kg.
5.3. Hm lng
C12H14O12Ca.2H2O
Khng thp hn 98,0% C12H14O12Ca.2H2O.
6. Phng php th
5.1. tinh khit
Florid
- Th theo JECFA monograph 1 - Vol. 4, phng php I.
Ch

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
C12H14O12Ca.2H2O.
iod
0,1
tng
ng
vi
PH LC 4
YU CU K THUT V PHNG PHP TH I VI ASCORBYL PALMITAT
1. Tn khc, ch s
Vitamin C palmitate
10,66
mg
INS 304
ADI = 1-1,25 mg/kg th trng
2. nh ngha
Tn ha hc
L-ascorbyl palmitat; Ascorbyl palmitat; Natri 2,3-didehydro-L-threohexono-1,4-lacton-6-palmitat; 6-palmitoyl-3-keto-L-gulofuranolacton.
Cng thc phn t
C22H38O7
Cng thc cu to
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
5.2. tinh khit

Khng c qu 2%.
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 mg/kg.
5.3. Hm lng C22H38O7
6. Phng php th
6.1. nh tnh
Phn ng kh
6.2. tinh khit


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


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.
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-L-threo-hexono1,4-lacton-6-stearat; 6-stearoyl-3-keto-L-gulofuranolacton.
Cng thc phn t
C24H42O7
M s C.A.S.
25395-66-8
Cng thc cu to
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
5.2. tinh khit

Khng c qu 2%.
Tro sulfat
Khng c qu 0,1%.
Ch
Khng c qu 2 mg/kg.
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

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

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

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.
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 Disoascorbic
M s C.A.S.
89-65-9
Cng thc phn t
C6H8O6
Cng thc cu to
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
5.2. tinh khit

Khng c qu 0,4%.
Gc quay cc ring
[]D25 trong khong -16,5o v -18,5o.
Tro sulfat
Khng c qu 0,3%.
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng C6H8O6
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.
6.2. tinh khit


- 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

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-alpha-tocopherol,

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
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
Khng tan trong nc, d tan trong ethanol, ha ln c vi ether.
Gc quay cc ring
20D : 00,05
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)
(dung dch 1/10 trong cloroform)
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
Ch
Khng c qu 2 mg/kg.
5.3. Hm lng dl-alphatocopherol
Khng c nh hn 96% v khng c qu 102%.
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

- 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 boro-silicat 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 240 oC 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 n-hexan 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 (alpha-tocopherol) 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 3,4,5trihydroxybenzoic, propyl 3,4,5-trihydroxybenzoat
M s C.A.S.
121-79-9
Cng thc ha hc
C10H12O5
Cng thc cu to
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 propan-1,2-diol.
Khong nng chy
146 150 oC sau khi lm kh.
Acid galic
Sc k lp mng-tch cc ester t yu cu (m t trong phn phng php th).

galat
5.2. tinh khit
Mt khi lng khi lm kh
Khng c qu 0,5%.
Tro sulfat
Khng c qu 0,1%
Hp cht hu c Clor ha
Khng c qu 100 mg/kg tnh theo clor.
Acid t do
Khng c qu 0,5% tnh theo acid galic.
Ch
Khng c qu 2 mg/kg.
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 ester Dng bn mng trng silica gel G. Chun b dung dch th bng cch
galat
ha tan 10 mg mu th trong 10 ml ethanol. 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.
5.2. tinh khit
Mt khi lng khi lm kh

- sy ti 110 C trong 4 gi.
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

- 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
2. nh ngha
L nha t g cy Guajacum officinale L., hoc cy Guajacum sanctum

L., (Fam. Zygophyllaceae), cha khong 70% acid alpha- v betaguaiaconic, 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
5.2. tinh khit

Tro ton phn
Khng c qu 5%.
Tro khng tan trong acid
Khng c qu 2%.
Cn khng tan trong ethanol Khng c qu 15%.

Rosin
Ch
Khng c qu 2 mg/kg.
6. Phng php th
5.1. 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.
5.2. 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

- 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

2. nh ngha
Tn ha hc
Mono-tert-butylhydroquinon; t-butylhydroquinon; 2-(1,1-dimethylethyl)-1,4benzendiol
M s C.A.S.
1948-33-0
Cng thc ha hc
C10H14O2
Cng thc cu to
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
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 mg/kg.
Ch
Khng c qu 2 mg/kg.
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 CaF 2
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 -tert-butyl-pbenzoquinon 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 / WU
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-dibutyl- Thit b:
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
Dung dch gc: cn chnh xc 50 mg hydroquinon (HQ), 50 mg 2,5-di-tbutylhydroquinon (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,O-bistrimethylsilylacetamid, 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 cell: 300 oC
t H2 v O2 (hoc khng kh) : 1,4 atm (20 Psi) cho mi kh
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

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 pdiphenylamin 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 C 10H14O2 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
2. nh ngha
Tn ha hc
3-Tert-butyl-4-hydroxyanisol;
hydroxyanisol
M s C.A.S.
25013-16-5
Cng thc ha hc
C11H16O2
hn
hp
ca
3-
2-tert-butyl-4-
Cng thc cu to
ng phn v tr 3
ng phn v tr 2
Khi lng phn t
180,25
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
5.2. tinh khit

Tro sulfat
Khng c qu 0,05%.
Ch
Khng c qu 2 mg/kg.
Tp cht phenol
Khng c qu 0,5%.
Khng thp hn 98,5% C 11H16O2 v khng thp hn 85% 3-tert-butyl-4hydroxyanisol.
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 2,6-dicloroquinonclorimid 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

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
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.
6.3. nh lng
Phng php sc k kh
Dung dch ni chun (c th tu chn Diphenylamin hoc 4-tertbutylphenol). 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-4-hydroxyanisol:
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
Kh mang: Nit, tc dng 30 ml/pht
B: iu kin cht ni chun ra gii ra trc 3-ter-butyl-4hydroxyanisol:
Ct: Ct thu tinh kch thc 2 m x 3 mm
Cht nhi: 5% Versamit-900 c ht 80/100 mesh cromosorb W-AWDMCS
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 3butyl 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
o
C; 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-4- hydroxyanisol v khng vt qu 6% vi ng phn 2tert-butyl-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
2. nh ngha
Tn ha hc
2,6-Ditertiary-butyl-p-cresol; 4-methyl-2,6-ditertiary-butyl-phenol
M s C.A.S.
128-37-0
Cng thc ha hc
C15H24O
Cng thc cu to
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
69o - 72oC
Quang ph
Phn ng mu
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 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 NaNO 2 (3/1000) v 5 ml dung dch dianisidin
dihydroclorid (Cn 200 mg 3,3-dimethoxy-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

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
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.
6.3. nh lng
Phng php sc k kh (JECFA monograph 1 - Vol. 4)

Dung dch ni chun: (cht ni chun tu chn diphenylamin hoc 4-tertbutylphenol). 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
o
C. 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
Didodecyl 3,3'-thiodipropionic; Ester Dilauryl ca acid ,'thiodipropionic
Ch s C.A.S.
123-28-4
Cng thc phn t
C30H58O4S
Cng thc cu to
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 - 215.
5.2. tinh khit

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

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 p-ethoxychrysoidin (TS) v chun ngay vi dung dch bromidbromat 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.

QCVN4 6 ChatChongOxiHoa

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

QCVN4 6 ChatChongOxiHoa

Uploaded by

Copyright:

Available Formats

CNG HO X HI CH NGHA VIT NAM

QCVN 4-6 : 2010/BYT

QUY CHUN K THUT QUC GIA

QUY CHUN K THUT QUC GIA

1.8. Ph lc 8: Yu cu k thut v phng php th i vi propyl galat.

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

Cng thc phn t

Khi lng phn t

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

Cht chng oxy ha

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

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

5.2. tinh khit

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

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

5.3. Hm lng C6H8O6

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

Ly 2 ml dung dch mu th 2,0% trong nc, thm 2 ml nc, 0,1 g

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

5.2. tinh khit

Gim khi lng khi lm kh

- Th theo JECFA monograph 1 - Vol. 4

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

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

Cng thc phn t

Khi lng phn t

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

Cht chng oxy ha

D tan trong nc, tan rt t trong ethanol.

Phi c phn ng c trng ca ascorbat.

Phi c phn ng c trng ca natri.

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

5.2. tinh khit

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

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

5.3. Hm lng C6H7O6Na

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

- Th theo JECFA monograph 1 - Vol. 4

Dung dch mu th s lm mt mu ca dung dch 2,6-diclorophenol

6.2. tinh khit

- Th theo JECFA monograph 1 - Vol. 4

- Th theo JECFA monograph 1 - Vol. 4.

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

Calci ascorbat dihydrat; Mui calci ca acid 2,3-didehydro-L-threohexono-1,4-lacton dehydrat.

Cng thc phn t

Khi lng phn t

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

Cht chng oxy ha

Phi c phn ng c trng ca calci.

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

5.2. tinh khit

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

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

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

- Th theo JECFA monograph 1 - Vol. 4.

Cn 0,4 g (chnh xc n mg) mu th cho vo bnh 250 ml, thm 50 ml

L-ascorbyl palmitat; Ascorbyl palmitat; Natri 2,3-didehydro-L-threohexono-1,4-lacton-6-palmitat; 6-palmitoyl-3-keto-L-gulofuranolacton.

Cng thc phn t

Khi lng phn t

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

Cht chng oxy ha

Rt t tan trong nc, d tan trong ethanol.

Khong nng chy