QUY CHUN K THUT QUC GIA V PH GIA THC PHM - CHT IU V

National technical regulation on Food additive Flavour enhancer

I. QUY NH CHUNG 1. Phm vi iu chnh Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc yu cu k thut v qun l v cht lng, v sinh an ton i vi cc cht iu v 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 iu v 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. Cc cht iu v: l ph gia thc phm c s dng vi mc ch tng hng v ca cc sn phm 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 iu v 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 LGlutamic

QCVN 4-1 : 2010/BYT

1.2. 1.3. 1.4. 1.5. 1.6. 1.7. 1.8. Ph lc 2: Ph lc 3: Ph lc 4: Ph lc 5: Ph lc 6: Ph lc 7: Ph lc 8: Yu cu k thut v phng php th i vi mononatri L-glutamat Yu cu k thut v phng php th i vi monokali L-glutamat Yu cu k thut v phng php th i vi calci di-Lglutamat Yu cu k thut v phng php th i vi acid 5'guanylic Yu cu k thut v phng php th i vi acid 5'inosinic Yu cu k thut v phng php th i vi maltol Yu cu k thut v phng php th i vi ethyl maltol

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 iu v 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 iu v Vic kim tra cht lng, v sinh an ton i vi cc cht iu v phi thc hin theo cc quy nh ca php lut.

QCVN 4-1 : 2010/BYT

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 iu v sau khi hon tt ng k bn cng b hp quy v bo m cht lng, v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut. V. T CHC THC HIN 1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chc nng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny. 2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhim kin ngh B Y t sa i, b sung Quy chun ny. 3. Trng hp hng dn ca quc t v phng php th v cc quy nh ca php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th th p dng theo vn bn mi.

QCVN 4-1 : 2010/BYT

Ph lc 1 YU CU K THUT V PHNG PHP TH I VI ACID L-GLUTAMIC 1. Tn khc, ch s L-glutamic acid, Glutamic acid INS 620 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to

HO NH2

Acid L-glutamic; Acid L-(+)-glutamic, acid L-2-aminopentandioic; Acid L-alpha-aminoglutaric 56-86-0 C5H9NO4
O H O OH

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Glutamat 5.2. tinh khit

147,13 Tinh th hoc bt tinh th mu trng, hoc khng mu. Cht iu v, thay th mui.

t tan trong nc, thc t khng tan trong ethanol v ether. Phi c phn ng c trng ca glutamat.

Gim khi lng khi lm Khng c qu 0,2% (Sy ti 80 oC trong 3 gi). kh pH Gc quay cc ring Tro sulfat Clorid Acid pyrrolidon carboxylic Arsen Dung dch bo ha mu th c pH trong khong 3,0 - 3,5. Dung dch mu th 10% (kl/tt) trong acid hydrocloric 2 N c [ ]D20 trong khong +31,5 n +32,2o Khng c qu 0,2%. Khng c qu 0,2%. t yu cu (m t trong phn phng php th). Khng c qu 3,0 mg/kg

QCVN 4-1 : 2010/BYT

Ch 5.3. Hm lng C5H9NO4 6. Phng php th 6.1 tinh khit Tro sulfat Clorid Th theo JECFA monograph 1 - Vol.4 - Phng php I, cn 1 g mu. Th theo JECFA monograph 1 - Vol.4 - Cn 0,07 g mu th, tin hnh theo hng dn trong chuyn lun th gii hn clorid, s dng 0,4 ml dung dch acid hydrocloric 0,01 N lm mu chng. - Th theo JECFA monograph 1 - Vol.4. Phng php sc k bn mng. - Mu th : Chun b dung dch mu th 0,5%. Ly 2 l. - Chun : pha dung dch chun mononatri glutamat 0,5% cha 2,5 mg acid pyrrolidon carboxylic. - Dung mi: hn hp n-butanol/acid acetic bng/nc, t l th tch 2/1/1. - Pha tnh hp ph : Silicagel. Dung dch h tinh bt-kali iodid : un nng 0,5 g tinh bt trong 50 ml nc khuy u n khi h ha. ngui, thm 0,5 g kali iodid v thm nc n 100 ml. - Tin hnh chy sc k theo hng dn trong chuyn lun sc k bn mng (cc phng php phn tch). Dng qu trnh sc k khi tuyn dung mi cch im xut pht khong 10 cm, kh dung mi trong khng kh, khong 30 pht. - ng thi, chun b bung sc k tng t, t vo 1 cc thy tinh dung tch 50 ml, cho vo cc 3 g natri hypoclorid, thm t t vo cc 1 ml acid hydrocloric to kh clor, y np v yn trong 30 giy to mi trng kh clor trong bung. t bn mng kh vo bung sc k, y np v yn trong 20 pht. Ly bn mng ra khi bung, yn 10 pht trong khng kh v xt ethanol ln bn mng. Sau khi kh, xt dung dch h tinh bt-kali iodid ln bn mng, quan st di nh sng thng ngay sau khi vt chun xut hin. Yu cu : Trong sc k ca mu th khng c c vt tng ng vt acid pyrrolidon carboxylic trong sc k ca chun ( nhy 0,2%). - Th JECFA monograph 1 - Vol.4, Phng php II. - 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 5 Khng c qu 1,0 mg/kg. Khng thp hn 99,0% tnh theo ch phm lm kh.

Acid pyrrolidon carboxylic

Arsen Ch

QCVN 4-1 : 2010/BYT

php chun b mu da trn nguyn tc ca phng php m t ti JECFA monograph 1 - Vol.4 phn cc phng php phn tch cng c. 6.2. nh lng Cn khong 200 mg (chnh xc n mg) mu th c lm kh trc, ha tan trong 6 ml acid formic, thm 100 ml acid acetic bng. Chun vi dung dch acid percloric 0,1 N, xc nh im kt thc chun bng o th. Tin hnh lm mu trng song song hiu chnh nn. Mi ml dung dch acid percloric 0,1 N tng ng vi 14,713 mg C5H9NO4.

QCVN 4-1 : 2010/BYT

Ph lc 2 YU CU K THUT V PHNG PHP TH I VI MONONATRI L-GLUTAMAT 1. Tn khc, ch s Monosodium L-glutamate, Sodium glutamate INS 621 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Mononatri L-glutamat monohydrat; Mui mononatri ca acid glutamic, monohydrat 6106-04-3 C5H8NNaO4.H2O

NH2 HO O O O
-

Na +

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Glutamat Natri 5.2. tinh khit Gim khi lng khi lm kh pH Gc quay cc ring Clorid Acid pyrrolidon carboxylic Ch

187,13 Tinh th hoc bt tinh th trng, thc t khng mi. Cht iu v.

D tan trong nc, t tan trong ethanol, thc t khng tan trong ether. Phi c phn ng c trng ca glutamat. Phi c phn ng c trng ca natri.

Khng c qu 0,5% (Sy ti 98oC trong 5 gi). Dung dch mu th 1/50 c pH trong khong 6,7 - 7,2. Dung dch mu th 10% (kl/tt) trong acid hydrocloric 2 N c [ ]D20 trong khong +24,8 n +25,3o Khng c qu 0,2%. t yu cu (m t trong phn phng php th). Khng c qu 1,0 mg/kg.

QCVN 4-1 : 2010/BYT

5.3. Hm lng C5H8NNaO4.H2O 6. Phng php th 6.1 tinh khit Clorid Th theo JECFA monograph 1 - Vol.4 - Cn 0,07 g mu th, tin hnh theo hng dn trong chuyn lun th gii hn clorid, s dng 0,4 ml dung dch acid hydrocloric 0,01 N lm mu chng. - Th theo JECFA monograph 1 - Vol.4. Phng php sc k bn mng. - Mu th : Chun b dung dch mu th 0,5%. Ly 2 l. - Chun : pha dung dch chun mono natri glutamat 0,5% cha 2,5 mg acid pyrrolidon carboxylic. - Dung mi: hn hp n-butanol/acid acetic bng/nc, t l th tch 2/1/1. - Pha tnh hp th : Silicagel. Dung dch h tinh bt-kali iodid : un nng 0,5 g tinh bt trong 50 ml nc khuy u n khi h ha. ngui, thm 0,5 g kali iodid v thm nc n 100 ml. - Tin hnh chy sc k theo hng dn trong chuyn lun sc k bn mng (cc phng php phn tch). Dng qu trnh sc k khi tuyn dung mi cch im xut pht khong 10 cm, kh dung mi trong khng kh, khong 30 pht. - ng thi, chun b bung sc k tng t, t vo 1 cc thy tinh dung tch 50 ml, cho vo cc 3 g natri hypoclorid, thm t t vo cc 1 ml acid hydrocloric to kh clor, y np v yn trong 30 giy to mi trng kh clor trong bung. t bn mng kh vo bung sc k, y np v yn trong 20 pht. Ly bn mng ra khi bung, yn 10 pht trong khng kh v xt ethanol ln bn mng. Sau khi kh, xt dung dch h tinh bt-kali iodid ln bn mng, quan st di nh sng thng ngay sau khi vt chun xut hin. Yu cu : Trong sc k ca mu th khng c c vt tng ng vt acid pyrrolidon carboxylic trong sc k ca chun ( nhy 0,2%). - 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 ti JECFA monograph 1 - Vol.4 phn cc phng php phn tch cng c. Khng thp hn 99,0% tnh theo ch phm lm kh.

Acid pyrrolidon carboxylic

Ch

6.2. nh lng Cn khong 200 mg (chnh xc n mg) mu th c 8

QCVN 4-1 : 2010/BYT

lm kh trc, ha tan trong 6 ml acid formic, thm 100 ml acid acetic bng. Chun vi dung dch acid percloric 0,1 N, xc nh im kt thc chun bng o th. Tin hnh lm mu trng song song hiu chnh nn. Mi ml dung dch acid percloric 0,1 N tng ng vi 9,356 mg C5H9NNaO4.H2O.

QCVN 4-1 : 2010/BYT

Ph lc 3 YU CU K THUT V PHNG PHP TH I VI MONOKALI L-GLUTAMAT 1. Tn khc, ch s Monopotassium L-glutamate, Potassium glutamate; MPG INS 622 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Monokali L-glutamat monohydrat; Mui monokali ca acid glutamic monohydrat 19473-49-5 C5H8NKO4.H2O

NH2 HO O O O
-

K+

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Glutamat Kali 5.2. tinh khit Gim khi lng khi lm kh pH Gc quay cc ring Clorid Acid pyrrolidon carboxylic Ch

203,24

Cht iu v, thay th mui.

D tan trong nc, t tan trong ethanol. Phi c phn ng c trng ca glutamat. Phi c phn ng c trng ca kali.

Khng c qu 0,2% (Sy ti 80oC trong 5 gi). Dung dch mu th 1/50 c pH trong khong 6,7 - 7,3. Dung dch mu th 10% (kl/tt) trong acid hydrocloric 2 N c [ ]D20 trong khong +22,5 n +24,0o Khng c qu 0,2%. t yu cu (m t trong phn phng php th). Khng c qu 1,0 mg/kg.

10

QCVN 4-1 : 2010/BYT

5.3. Hm lng C5H8NKO4.H2O 6. Phng php th 6.1 tinh khit Clorid - Th theo JECFA monograph 1 - Vol.4 - Cn 0,07 g mu th, tin hnh theo hng dn trong chuyn lun th gii hn clorid, s dng 0,4 ml dung dch acid hydrocloric 0,01 N lm mu chng. - Th theo JECFA monograph 1 - Vol.4. Phng php sc k bn mng. - Mu th : Chun b dung dch mu th 0,5%. Ly 2 l. - Chun : pha dung dch chun mono natri glutamat 0,5% cha 2,5 mg acid pyrrolidon carboxylic. - Dung mi: hn hp n-butanol/acid acetic bng/nc, theo t l th tch tng ng 2/1/1. - Pha tnh hp th : Silicagel. Dung dch h tinh bt-kali iodid : un nng 0,5 g tinh bt trong 50 ml nc khuy u n khi h ha. ngui, thm 0,5 g kali iodid v thm nc n 100 ml. - Tin hnh chy sc k theo hng dn trong chuyn lun sc k bn mng (cc phng php phn tch). Dng qu trnh sc k khi tuyn dung mi cch im xut pht khong 10 cm, kh dung mi trong khng kh, khong 30 pht. - ng thi, chun b bung sc k tng t, t vo 1 cc thy tinh dung tch 50 ml, cho vo cc 3 g natri hypoclorid, thm t t vo cc 1 ml acid hydrocloric to kh clor, y np v yn trong 30 giy to mi trng kh clor trong bung. t bn mng kh vo bung sc k, y np v yn trong 20 pht. Ly bn mng ra khi bung, yn 10 pht trong khng kh v xt ethanol ln bn mng. Sau khi kh, xt dung dch h tinh bt-kali iodid ln bn mng, quan st di nh sng thng ngay sau khi vt chun xut hin. Yu cu : Trong sc k ca mu th khng c c vt tng ng vt acid pyrrolidon carboxylic trong sc k ca chun ( nhy 0,2%). - 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 ti JECFA monograph 1 - Vol.4 phn cc phng php phn tch cng c. Khng thp hn 99,0% tnh theo ch phm lm kh.

Acid pyrrolidon carboxylic

Ch

11

QCVN 4-1 : 2010/BYT

6.2. nh lng Cn khong 200 mg (chnh xc n mg) mu th c lm kh trc, ha tan trong 6 ml acid formic, thm 100 ml acid acetic bng. Chun vi dung dch acid percloric 0,1 N, xc nh im kt thc chun bng o th. Tin hnh lm mu trng song song hiu chnh nn Mi ml dung dch acid percloric 0,1 N tng ng vi 10,162 mg C5H8KNO4.H2O.

12

QCVN 4-1 : 2010/BYT

Ph lc 4 YU CU K THUT V PHNG PHP TH I VI CALCI di-L-GLUTAMAT 1. Tn khc, ch s Monocalcium di-L-glutamate, Calcium glutamate; INS 623 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Monocalci di-L-glutamat; 19238-49-4 C10H16CaN2O8 . xH2O (x = 0, 1, 2, 6 hoc 4)

NH2 HO O O 2 O
-

Ca + +

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Glutamat Calci 5.2. tinh khit Nc Gc quay cc ring Clorid Acid pyrrolidon carboxylic Ch 5.3. Hm lng C10H16CaN2O8

332,32 (dng khan) Tinh th hoc bt tinh th trng, thc t khng mi. Cht iu v, thay th mui.

D tan trong nc. Phi c phn ng c trng ca glutamat. Phi c phn ng c trng ca calci.

Khng c qu 19,0% Dung dch mu th 10% (kl/tt) trong acid hydrocloric 2 N c [ ]D20 trong khong +27,4 n +29,2o Khng c qu 0,2%. t yu cu (m t trong phn phng php th). Khng c qu 1,0 mg/kg. Khng thp hn 98,0% v khng c qu 102,0% tnh theo ch phm khan.

13

QCVN 4-1 : 2010/BYT

6. Phng php th 6.1 tinh khit Nc - Th theo JECFA monograph 1 - Vol.4 - Phng php Karl Fischer. Clorid - Th theo JECFA monograph 1 - Vol.4 - Cn 0,07 g mu th, tin hnh theo hng dn trong chuyn lun th gii hn clorid, s dng 0,4 ml dung dch acid hydrocloric 0,01 N lm mu chng. Acid pyrrolidon carboxylic - Th theo JECFA monograph 1 - Vol.4. Phng php sc k bn mng. - Mu th : Chun b dung dch mu th 0,5%. Ly 2 l. - Chun : pha dung dch chun mono natri glutamat 0,5% cha 2,5 mg acid pyrrolidon carboxylic. - Dung mi: hn hp n-butanol/acid acetic bng/nc, t l th tch 2/1/1. - Pha tnh hp th : Silicagel. Dung dch h tinh bt-kali iodid : un nng 0,5 g tinh bt trong 50 ml nc khuy u n khi h ha. ngui, thm 0,5 g kali iodid v thm nc n 100 ml. - Tin hnh chy sc k theo hng dn trong chuyn lun sc k bn mng (cc phng php phn tch). Dng qu trnh sc k khi tuyn dung mi cch im xut pht khong 10 cm, kh dung mi trong khng kh, khong 30 pht. - ng thi, chun b bung sc k tng t, t vo 1 cc thy tinh dung tch 50 ml, cho vo cc 3 g natri hypoclorid, thm t t vo cc 1 ml acid hydrocloric to kh clor, y np v yn trong 30 giy to mi trng kh clor trong bung. t bn mng kh vo bung sc k, y np v yn trong 20 pht. Ly bn mng ra khi bung, yn 10 pht trong khng kh v xt ethanol ln bn mng. Sau khi kh, xt dung dch h tinh bt-kali iodid ln bn mng, quan st di nh sng thng ngay sau khi vt chun xut hin. Yu cu : Trong sc k ca mu th khng c c vt tng ng vt acid pyrrolidon carboxylic trong sc k ca chun ( nhy 0,2%). - 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 ti JECFA monograph 1 - Vol.4 phn cc phng php phn tch cng c.

Ch

14

QCVN 4-1 : 2010/BYT

6.2. nh lng Cn khong 250 mg (chnh xc n mg) mu th c lm kh trc, ha tan trong 6 ml acid formic, thm 100 ml acid acetic bng. Chun vi dung dch acid percloric 0,1 N, xc nh im kt thc chun bng o th. Tin hnh lm mu trng song song hiu chnh nn Mi ml dung dch acid percloric 0,1 N tng ng vi 8,308 mg C10H16CaN2O8. Tnh hm lng da trn ch phm khan.

15

QCVN 4-1 : 2010/BYT

Ph lc 5 YU CU K THUT V PHNG PHP TH I VI ACID 5-GUANYLIC 1. Tn khc, ch s 5-Guanylic acid; Guanylic acid; GMP INS 626 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Acid Guanosin-5-monophosphoric 85-32-5 C10H14N5O8P

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Ph hp th quang

363,22 Tinh th trng hoc khng mu, bt tinh th trng; khng mi Cht iu v

t tan trong nc, thc t khng tan trong ethanol. Dung dch mu th 1/50000 trong acid hydrocloric 0,01 N c cc i hp th ti 256 2 nm. T s A256/A260 trong khong t 0,95 n 1,03 v t s A280/A260 trong khong t 0,63 n 0,71. Phi c phn ng c trng ca ribose. Phi c phn ng c trng ca phosphat hu c.

Ribose Phosphat hu c 5.2. tinh khit Gim khi lng khi lm kh pH

Khng c qu 1,5% (sy 120 oC trong 4 gi). Dung dch mu th 1/400 c pH t 1,5 n 2,5 .

16

QCVN 4-1 : 2010/BYT

Cc tp cht ngoi lai c lin quan Ch 5.3. Hm lng C10H14N5O8P 6. Phng php th 6.1. nh tnh Phosphat hu c 6.2. tinh khit Cc tp cht ngoi lai c lin quan Ch - Th theo hng dn ti JECFA monograph 1 - Vol.4 - dng 2 l dung dch mu th 1/400. 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 ti JECFA monograph 1 - Vol.4 phn cc phng php phn tch cng c. - Th theo hng dn ti JECFA monograph 1 - Vol.4 - Dch th l dung dch mu th 1/400. Khng pht hin bng phng php sc k. Khng c qu 1,0 mg/kg. Khng thp hn 97,0% v khng c qu 102,0% tnh theo ch phm lm kh.

6.3. nh lng Cn khong 0,5 g (chnh xc n 0,1 mg) mu th ha tan trong acid hydrocloric 0,01 N v nh mc n 1000 ml. ly 10 ml dung dch ny pha long vi acid hydrocloric 0,01 N va thu c 250 ml. Xc nh hp th quang ca dung dch ny trong cuvet 1 cm ti bc sng 260 nm v s dng dung dch acid hydrocloric 0,01 N lm mu chng. Tnh hm lng % C10H14N5O8P trong mu th theo cng thc sau: A X 235
X 100 100 100- gim khi lng khi lm kh (%)

%=

250000 Khi lng mu (mg)

17

QCVN 4-1 : 2010/BYT

Ph lc 6 YU CU K THUT V PHNG PHP TH I VI ACID 5-INOSINIC 1. Tn khc, ch s 5- Inosinic acid; Inosinic acid; IMP INS 630 ADI khng gii hn

2. nh ngha Tn ha hc M s C.A.S. Cng thc phn t Cng thc cu to Acid Inosin-5-monophosphoric 131-99-7 C10H13N4O8P

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Ph hp th quang

348,21 Tinh th trng hoc khng mu, bt tinh th trng; khng mi Cht iu v

D tan trong nc, t tan trong ethanol. Dung dch mu th 1/50000 trong acid hydrocloric 0,01 N c cc i hp th ti 250 2 nm. T s A250/A260 trong khong t 1,55 n 1,65 v t s A280/A260 trong khong t 0,20 n 0,30. Phi c phn ng c trng ca ribose. Phi c phn ng c trng ca phosphat hu c.

Ribose Phosphat hu c 5.2. tinh khit Gim khi lng khi lm kh pH Cc tp cht ngoi lai c lin quan

Khng c qu 3,0% (sy ti 120 oC trong 4 gi). Dung dch mu th 1/20 c pH t 1,0 n 2,0. Khng pht hin bng phng php sc k.

18

QCVN 4-1 : 2010/BYT

Ch 5.3. Hm lng C10H13N4O8P 6. Phng php th 6.1. nh tnh Phosphat hu c 6.2. tinh khit Cc tp cht ngoi lai c lin quan Ch - Th theo hng dn ti JECFA monograph 1 - Vol.4 - dng 1 l dung dch mu th 1/200. - 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. - Th theo hng dn ti JECFA monograph 1 - Vol.4 - Dch th l dung dch mu th 1/400. Khng c qu 1,0 mg/kg. Khng thp hn 97,0% v khng c qu 102,0% tnh theo ch phm lm kh.

6.3. nh lng Cn khong 0,5 g (chnh xc n 0,1 mg) mu th ha tan trong acid hydrocloric 0,01 N v nh mc n 1000 ml. ly 10 ml dung dch ny pha long vi acid hydrocloric 0,01 N va thu c 250 ml. Xc nh hp th quang ca dung dch trong cuvet 1 cm ti bc sng 250 nm v s dng dung dch acid hydrocloric 0,01 N lm mu chng. Tnh hm lng % C10H13N4O8P trong mu th theo cng thc sau: A 349 250000 Khi lng mu (mg) 100 100- gi tr gim khi lng khi lm kh (%)

%=

100

19

QCVN 4-1 : 2010/BYT

Ph lc 7 YU CU K THUT V PHNG PHP TH I VI MALTOL 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 636 ADI = 0 - 1 mg/kg th trng Maltol thu c bng cch tng hp ha hc 3-hydroxy-2-methyl-4-pyron 118-71-8 C6H6O3

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Khong nng chy Hp th t ngoi 5.2. tinh khit Nc Tro sulfat Ch 5.3. Hm lng C6H6O3 6. Phng php th 6.1. tinh khit Nc Tro sulfat

126,11 Bt tinh th trng c mi caramel b ngo ng. Cht iu v, tr hng, hng liu.

t tan trong nc, tan trong ethanol v propylen glycol. 160o - 164o. Ph hp th t ngoi ca dung dch mu th 10 mg/l trong acid hydrocloric 0,1 N c 1 cc i hp th ti 274 nm.

Khng c qu 0,5% Khng c qu 0,2%. (Cn 5 g mu). Khng c qu 1,0 mg/kg. Khng thp hn 99,0% tnh theo ch phm khan.

- Th theo hng dn ti JECFA monograph 1 - Vol.4. - Phng php Karl-Fischer. - Th theo hng dn ti JECFA monograph 1 - Vol.4. 20

QCVN 4-1 : 2010/BYT

- Mu th: Cn 5 g . Ch - Th theo hng dn ti JECFA monograph 1 - Vol.4. - Xc nh bng k thut AAS-ICP/AES 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 ti JECFA monograph 1 - Vol.4 phn Cc phng php chung, tp cht kim loi.

6.2. nh lng Dung dch chun Cn 50 mg (chnh xc) chun Maltol USP, cho vo bnh nh mc 250 ml, ha tan v nh mc n vch bng acid hydrocloric 0,1 N v lc u. Dng pipet ly 5 ml cho vo bnh nh mc 100 ml, pha long n vch bng acid hydrocloric 0,1 N, lc u. Dung dch nh lng Cn 50 mg (chnh xc) mu th, cho vo bnh nh mc 250 ml, ha tan v nh mc n vch bng acid hydrocloric 0,1 N v lc u. Dng pipet ly 5 ml cho vo bnh nh mc 100 ml, pha long n vch bng acid hydrocloric 0,1 N, lc u. Tin hnh th Xc nh hp th quang ca dung dch chun v dung dch nh lng ti 274 nm s dng cuvet o 1 cm bng thch anh, acid hydrocloric 0,1 N l mu trng. Tnh hm lng % ca maltol trong mu th theo cng thc sau: % Maltol = 100 x W S x AA / (AS x WA) Trong : AA l hp th quang ca dung dch mu (dung dch nh lng) AS l hp th quang ca dung dch chun WA l khi lng mu trong dung dch nh lng (mg) WS l khi lng chun trong dung dch chun (mg)

21

QCVN 4-1 : 2010/BYT

Ph lc 8 YU CU K THUT V PHNG PHP TH I VI ETHYL MALTOL 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 637 ADI = 0 - 2 mg/kg th trng Ethyl maltol thu c bng cch tng hp ha hc 2-Ethyl-3-hydroxy-4-pyron 4940-11-8 C7H8O3

Khi lng phn t 3. Cm quan 4. Chc nng 5. Yu cu k thut 5.1. nh tnh tan Khong nng chy Hp th t ngoi 5.2. tinh khit Nc Tro sulfat Ch 5.3. Hm lng C7H8O3 6. Phng php th 6.1 tinh khit Nc Tro sulfat

140,14 Bt tinh th trng c mi ko bng. Cht iu v, tr hng, hng liu.

t tan trong nc, tan trong ethanol v propylen glycol. 89o - 93o. Ph hp th t ngoi ca dung dch mu th 10 mg/l trong acid hydrocloric 0,1 N c 1 cc i hp th ti 276 nm.

Khng c qu 0,5% . Khng c qu 0,2%. Khng c qu 1,0 mg/kg. Khng thp hn 99,0% tnh theo ch phm khan.

- Th theo hng dn ti JECFA monograph 1 - Vol.4 - Phng php Karl Fischer - Th theo hng dn ti JECFA monograph 1 - Vol.4 22

QCVN 4-1 : 2010/BYT

- Cn 5 g mu Ch - Th theo hng dn ti JECFA monograph 1 - Vol.4. - Xc nh bng k thut AAS-ICP/AES 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 ti JECFA monograph 1 - Vol.4 phn Cc phng php chung, tp cht kim loi.

6.2. nh lng Dung dch chun Cn 50 mg (chnh xc) chun Ethyl maltol USP, cho vo bnh nh mc 250 ml, ha tan v pha long n vch bng acid hydrocloric 0,1 N v lc u. Dng pipet ly 5 ml cho vo bnh nh mc 100 ml, pha long n vch bng acid hydrocloric 0,1 N, lc u. Dung dch mu th Cn 50 mg (chnh xc) mu th, cho vo bnh nh mc 250 ml, ha tan v pha long n vch bng acid hydrocloric 0,1 N v lc u. Dng pipet ly 5 ml cho vo bnh nh mc 100 ml, pha long n vch bng acid hydrocloric 0,1 N, lc u. Tin hnh th Xc nh hp th quang ca dung dch chun v dung dch mu th ti 276 nm s dng cuvet o 1-cm bng thch anh, acid hydrocloric 0,1 N l mu trng. Tnh hm lng % ca Ethyl maltol trong mu th theo cng thc sau: % Ethyl maltol = 100 x W S x AA / (AS x W A) Trong : AA l hp th quang ca dung dch mu th AS l hp th quang ca dung dch chun WA l khi lng mu trong dung dch nh lng (mg) WS l khi lng chun trong dung dch chun (mg)

23