B Y T _________ S: 23/2010/TT-BYT

CNG HO X HI CH NGHA VIT NAM c lp - T do - Hnh phc __________________________ H Ni, ngy 20 thng 5 nm 2010

THNG T Ban hnh Quy chun k thut quc gia v ph gia thc phm - cht chng oxy ho ______________ B TRNG B Y T Cn c Lut Tiu chun v Quy chun k thut ngy 29 thng 6 nm 2006 v Ngh nh s 127/2007/N-CP ngy 01 thng 8 nm 2007 ca Chnh ph quy nh chi tit thi hnh mt s iu ca Lut Tiu chun v Quy chun k thut; Cn c Php lnh V sinh an ton thc phm ngy 07 thng 8 nm 2003 v Ngh nh s 163/2004/N-CP ngy 07 thng 9 nm 2004 ca Chnh ph quy nh chi tit thi hnh mt s iu ca Php lnh V sinh an ton thc phm; Cn c Ngh nh s 188/2007/N-CP ngy 27 thng 12 nm 2007 ca Chnh ph quy nh chc nng, nhim v, quyn hn v c cu t chc ca B Y t; Theo ngh ca Cc trng Cc An ton v sinh thc phm, V trng V Khoa hc v o to, V trng V Php ch, QUY NH: iu 1. Ban hnh km theo Thng t ny: QCVN 4-6: 2010/BYT - Quy chun k thut quc gia v ph gia thc phm Cht chng oxy ho. iu 2. Thng t ny c hiu lc t ngy 01 thng 01 nm 2011. iu 3. Cc trng Cc An ton v sinh thc phm, Th trng cc n v thuc B Y t, cc n v trc thuc B Y t; Gim c S Y t cc tnh, thnh ph trc thuc trung ng v cc t chc, c nhn c lin quan chu trch nhim thi hnh Thng t ny./. Ni nhn:
- VPCP (Vn x, Cng bo, Cng TTT Chnh ph); - Cc B, c quan ngang B, c quan thuc CP; - B T php (Cc Kim tra VBQPPL); - B trng Nguyn Quc Triu ( bo co); - UBND cc tnh, thnh ph trc thuc TW; - Vin Kim st nhn dn ti cao; - To n nhn dn ti cao; - S Y t cc tnh, thnh ph trc thuc TW; - Chi cc ATTP cc tnh, thnh ph trc thuc TW; - TTYTDP cc tnh, thnh ph trc thuc TW; - Cc c quan KTNN v thc phm nhp khu; - Tng Cc Tiu chun - o lng - Cht lng; - Website B Y t; - Lu: VT, K2T, PC, ATTP.

KT. B TRNG TH TRNG TH TRNG

Trnh Qun Hun

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 HO 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 HO 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 ho 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 ho 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 ho: l ph gia thc phm c s dng vi mc ch chng li s h hng ca thc phm do b oxy ho (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 2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Vitamin C INS 300 ADI khng gii hn L-ascorbic acid; ascorbic acid; 2,3-didehydro-L-threo-hexono1,4-lacton; 3-keto-L-gulouranolacton 50-81-7 C6H8O6

Khi lng phn t 3. Cm quan

4. Chc nng 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 Khng c qu 0,4%. kh 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 2,6-diclorophenol indophenol (TS). 5.2. tinh khit Gim khi lng khi lm - Th theo JECFA monograph 1 - Vol. 4 kh - 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

176,13 Bt tinh th trng hoc hi vng, khng mi, im nng chy khong 190 oC km theo phn hy. Cht chng oxy ha

6.3. nh lng

cng c). 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 2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to INS 301 ADI khng gii hn Natri L-ascorbat; Natri ascorbat; Natri 2,3-didehydro-L-threohexono-1,4-lacton enolat; Natri 3-keto-L-gulofuranolacton enolat. 134-03-2 C6H7O6Na

Khi lng phn t 3. Cm quan

4. Chc nng 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 Khng c qu 0,25%. kh 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 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 - Th theo JECFA monograph 1 - Vol. 4 kh - 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

198,11 Bt tinh th trng hoc gn nh trng, khng mi, s b sm mu khi ngoi nh sng. Cht chng oxy 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 2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to INS 302 ADI khng gii hn Calci ascorbat dihydrat; Mui calci ca acid 2,3-didehydro-Lthreo-hexono-1,4-lacton dehydrat. 5743-27-1 C12H14O12Ca.2H2O

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Calci Gc quay cc ring

426,35 Bt tinh th khng mi, mu trng hoc hi vng. Cht chng oxy ha Tan trong nc, rt t tan trong ethanol, khng tan trong ether. Phi c phn ng c trng ca calci. 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 Khng thp hn 98,0% C12H14O12Ca.2H2O. C12H14O12Ca.2H2O 6. Phng php th 5.1. 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 2. nh ngha Tn ha hc Cng thc phn t Cng thc cu to Vitamin C palmitate INS 304 ADI = 1-1,25 mg/kg th trng L-ascorbyl palmitat; Ascorbyl palmitat; Natri 2,3-didehydro-Lthreo-hexono-1,4-lacton-6-palmitat; 6-palmitoyl-3-keto-Lgulofuranolacton. C22H38O7

Khi lng phn t 3. Cm quan

4. Chc nng 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 Khng c qu 2%. kh 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 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 - Th theo JECFA monograph 1 - Vol. 4 kh - 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

414,55 Dng rn mu trng n trng vng, c mi ging qu h cam, chanh. Cht chng oxy ha

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 2. nh ngha Tn ha hc Cng thc phn t M s C.A.S. Cng thc cu to Vitamin C stearate INS 305 ADI = 1 - 1,25 mg/kg th trng L-ascorbyl stearat; Ascorbyl stearat; Natri 2,3-didehydro-Lthreo-hexono-1,4-lacton-6-stearat; 6-stearoyl-3-keto-Lgulofuranolacton. C24H42O7 25395-66-8

Khi lng phn t 3. Cm quan

4. Chc nng 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 Khng c qu 2%. kh Tro sulfat Khng c qu 0,1%. Ch Khng c qu 2 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 - Th theo hng dn ti JECFA monograph 1 - Vol. 4 kh - 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.

442,6 Dng rn mu trng n trng vng, c mi ging qu h cam, chanh Cht chng oxy ha

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 2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Acid erythorbic, Acid D-araboascorbic INS 315 ADI khng gii hn Acid D-erythro-hex-2-enoic deltalacton, Acid isoascorbic, Acid D- isoascorbic 89-65-9 C6H8O6

Khi lng phn t 3. M t 4. Chc nng 5. Tnh cht 5.1. nh tnh tan Khong nng chy Th ascorbat Phn ng kh 5.2. tinh khit Gim khi lng khi lm kh Gc quay cc ring Tro sulfat Ch 5.3. Hm lng C6H8O6 6. Phng php th 6.1. nh tnh Phn ng kh

176,13 Dng tinh th trng hoc hi vng, ng mu sm khi ngoi nh sng. Cht chng oxy ha D tan trong nc, tan trong ethanol. Khong 164 oC - 172oC, km theo phn hy. Phi c phn ng c trng ca ascorbat. t yu cu (m t trong phn phng php th). Khng c qu 0,4%. [ ]D25 trong khong -16,5o v -18,5o. Khng c qu 0,3%. Khng c qu 2 mg/kg. Khng thp hn 99,0% tnh theo ch phm lm 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). - Th theo JECFA monograph 1 - Vol. 4 - Lm kh di p sut gim, trn silicagel v trong 3 gi. - Th theo JECFA monograph 1 - Vol.4, Phng php I. - Cn 1g mu th. - 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). 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

6.2. tinh khit Gim khi lng khi lm kh Tro sulfat Ch

6.3. nh lng

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. dl-5,7,8-Trimethyltocol, dl-2,5,7,8-tetramethyl-2-(4',8',12'trimethyltridecyl)-6-cromanol 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. C29H50O2

2. nh ngha Tn ha hc M s C.A.S.

Cng thc ha hc Cng thc cu to

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Gc quay cc ring Quang ph Phn ng mu 5.2. tinh khit Ch s khc x Quang ph

430,71 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) Cht chng oxy ha Khng tan trong nc, d tan trong ethanol, ha ln c vi ether. : 00,05o (dung dch 1/10 trong cloroform) Dung dch trong ethanol tuyt i c cc i hp th khong 292 nm. t yu cu (m t trong phn phng php th)

n (20, D): 1,503 - 1,507 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 mg/kg. 5.3. Hm lng dl-alpha- Khng c nh hn 96% v khng c qu 102%. tocopherol 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

Ch

6.3. nh lng

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. - 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. 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 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 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 2. nh ngha Tn ha hc M s C.A.S. Cng thc ha hc Cng thc cu to INS 310 ADI = 0 1,4 mg/kg th trng Propyl galat, ester propyl ca acid gallic, ester n-propyl ca acid 3,4,5-trihydroxybenzoic, propyl 3,4,5-trihydroxybenzoat 121-79-9 C10H12O5

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 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 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. 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 ester galat cch 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 - Th theo JECFA monograph 1 - Vol. 4 - 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 - 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 2. nh ngha Gm Guaiac, Gum Guaiac, Gum Guaiacum, Guaiacum INS 314 ADI = 0 - 2,5 mg/kg th trng 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... 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. Cht chng oxy ha Khng tan trong nc, tan trong cht bo, d tan nhng tan khng hon ton trong ethanol, ether v dung dch kim. 85 90 oC. t yu cu (m t trong phn phng php th).

3. Cm quan

4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan

Khong nng chy 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 Khng c qu 15%. ethanol Rosin t yu cu (m t trong phn phng php th). 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 Cn 2 g (chnh xc n mg) mu th c nghin mn cho vo ethanol 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 TERTBUTYLHYDROQUINON 1. Tn khc, ch s 2. nh ngha Tn ha hc M s C.A.S. Cng thc ha hc Cng thc cu to Tertiary butylhydroquinone; TBHQ INS 319 ADI = 0 - 0,7 mg/kg th trng Mono-tert-butylhydroquinon; dimethylethyl)-1,4-benzendiol 1948-33-0 C10H14O2 t-butylhydroquinon; 2-(1,1-

Khi lng phn t 3. M t 4. Chc nng 5. Tnh cht 5.1. nh tnh tan im nng chy Cc phenol 5.2. tinh khit t-Butyl-p-benzoquinon 2,5-Dibutyl-hydroquinon Hydroquinon Toluen Ch 5.3. Hm lng C10H14O2 6. Phng php th 6.1. nh tnh Cc phenol 6.2. tinh khit t-Butyl-p-benzoquinon

166,22 Tinh th mu trng c mi c trng nh. Cht chng oxy ha Thc t khng tan trong nc, tan trong ehanol. Khng thp hn 126,5oC. t yu cu (m t trong phn phng php th). Khng c qu 0,2%. Khng c qu 0,2%. Khng c qu 0,1%. Khng c qu 25 mg/kg. Khng c qu 2 mg/kg. Khng thp hn 99,0% C10H14O2. 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. 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/ 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- 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,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

Toluen

Ch

6.3. nh lng

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). 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 - 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). 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-butylhydro- quinon (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 2. nh ngha Tn ha hc M s C.A.S. Cng thc ha hc Cng thc cu to Butylated hydroxyanisole; BHA INS 320 ADI = 0 - 0,5 mg/kg th trng 3-Tert-butyl-4-hydroxyanisol; hn hp ca 3- v 2-tert-butyl-4hydroxyanisol 25013-16-5 C11H16O2

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Phn ng mu 5.2. tinh khit Tro sulfat Ch Tp cht phenol 5.3. Hm lng C11H16O2 6. Phng php th 6.1. nh tnh Phn ng mu

ng phn v tr 3 ng phn v tr 2 180,25 Cht rn dng sp hoc tinh th mu trng hoc vng nht, c mi c trng nh. Cht chng oxy ha Khng tan trong nc, d tan trong propan-1,2-diol v ethanol. t yu cu (m t trong phn phng php th). Khng c qu 0,05%. Khng c qu 2 mg/kg. Khng c qu 0,5%. Khng thp hn 98,5% C11H16O2 v khng thp hn 85% 3-tertbutyl-4-hydroxyanisol. 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. - Th theo JECFA monograph 1 - Vol. 4, Phng php I. - Cn 5 g mu. - 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. - 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

6.2. tinh khit Tro sulfat Ch

Tp cht phenol

6.3. nh lng

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 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-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-butyl-4hydroxyanisol: Ct: Ct thu tinh kch thc 2 m x 3 mm Cht nhi: 5% Versamit-900 c ht 80/100 mesh cromosorb WAW- 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 2v 3- butyl hydroxy anisol. Tng hm lng ng phn 2- v 3chnh 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-

4- hydroxyanisol 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 2. nh ngha Tn ha hc M s C.A.S. Cng thc ha hc Cng thc cu to BHT INS 321 ADI = 0 - 0,3 mg/kg th trng 2,6-Ditertiary-butyl-p-cresol; 4-methyl-2,6-ditertiary-butyl-phenol 128-37-0 C15H24O

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Khong nng chy Quang ph Phn ng mu 5.2. tinh khit Nhit ng c Tro sulfat Ch Tp cht phenol 5.3. Hm lng C15H24O 6. Phng php th 6.1. nh tnh Quang ph Phn ng mu

220,36 Cht rn dng vy hoc tinh th mu trng, khng mi hoc c mi thm nh c trng. Cht chng oxy ha Khng tan trong nc v propan-1,2-diol, d tan trong ethanol. 69o - 72oC t yu cu (m t trong phn phng php th). t yu cu (m t trong phn phng php th). Khng c thp hn 69,2 oC. Khng c qu 0,005%. Khng c qu 2 mg/kg. Khng c qu 0,5%. Xem hng dn trong phn phng php th Khng thp hn 99,0%. 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. 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 3,3-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. - Th theo JECFA monograph 1 - Vol. 4, Phng php I. - Cn 20 g mu. - 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. tinh khit Tro sulfat Ch

Tp cht phenol

6.3. nh lng

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. 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 13 YU CU K THUT V PHNG PHP TH I VI DILAURRYL THIODIPROPIONAT 1. Tn khc, ch s 2. nh ngha Tn ha hc Ch s C.A.S. Cng thc phn t Cng thc cu to Dilauryl thiodipropionate INS 389 ADI = 0 - 3 mg/kg th trng Ester ca acid thiodipropionic v lauryl alcohol thc phm Didodecyl 3,3'-thiodipropionic; Ester Dilauryl ca acid , 'thiodipropionic 123-28-4 C30H58O4S

Khi lng phn t 3. M t 4. Chc nng 5. Tnh cht 5.1. nh tnh tan im ng c Ch s x phng ha 5.2. tinh khit Acid Ch 5.3. Hm lng C30H58O4S 6. Phng php th 6.1. tinh khit Tnh acid

514,86 Tinh th dng vy mu trng, c mi c trng ging ester ngt. Cht chng oxy ha. Khng tan trong nc, tan trong ethanol v ete. Khng thp hn 40o. 205 - 215. Khng c qu 0,2% (tnh theo acid thiodipropionic). Khng c qu 2 mg/kg. Khng thp hn 99,0%. 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. - 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). 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 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.

Ch

6.2. nh lng

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.