TIU CHUN VIT NAM

TCVN 5147:1990
THT V SN PHM CA THT. PHNG PHP XC NH D LNG PENIXILIN Meat and meat products. Determination of penicillin residues Tiu chun ny quy nh phng php xc nh tng penicillin tn d trong tht v sn phm ca tht dng lm thc phm cho ngi v thc n gia sc. 1 c tnh chung Penicillin thuc h khng sinh, l cht hu c c phn t lng ln, tn ti trong tht v sn phm ca tht vi hm lng rt nh. H penicillin gm nhiu dn xut nh benzyl penicillin, potasium penicillin, phenoxymethyl penicillin, ampycillin, anhydrous, bezathyl penicillin G, procaine penicillin G, v.v 2 Nguyn tc Ap dng phng php gin tip, da vo phn ng to phc c trng v hon ton nh lng ca penicillin vi thuc th phenaltrolin- cadimi sinh ra phc bn. Chit phc ny bng nitrobenzen v o ph hp th nguyn t ca kim loi cadimi trong phc tng hu c, hay phn hy tng hu c, ly cadimi vo axit clohydric, dung dch 1% v do ph ca caidimi. 3 Ly mu Theo TCVN 4833 - 89 ( ST SEV 2433 - 80) 4 Dng c, thit b v ho cht 4.1 Dng c, thit b: + My ph hp th nguyn t SP - 9/800 hay loi tng ng. + n catt rng ca cadimi + Bp un cch thy + My xay sinh t + Bnh nh mc cc loi + Pipet cc loi + Cc chu nhit + Phu chit 250 ml. + Mt s dng c khc 4.2 Ha cht: Dng loi tinh khit cao 99,99% hay tinh khit quang ph ( Specpure). + Thuc th Tris ( 1,10 - Phenaltrolin) Cadimi + Dung mi nitrobenzen ( C6H5NO2) + Dung dch gc tiu chun ca cadimi nng 1mg/ ml + Axit nitric, dung dch 65% + Hydroperoxyt (H2O2) dung dch 30% + Dung dch 1% ca 2 axitclohydric v nitric trong nc + Nc ct 2 ln. 5 Chun b th 5.1 Chun b mu phn tch:

Mu tht cn phn tch c thi nh, trn u, cn 1 lng 10 g cho vo my xay sinh t. Thm vo 30 ml nc ct ri cho my chy trong 5 pht. Cho ton b huyn dch vo cc chu nhit, iu chnh pH khong 5 - 6 ri un cch thy 60 - 70 0 C trong 30 pht. Chuyn dung dch ny vo bnh nh mc v nh mc bng nc ct n th tch 50 ml. Sau ly tm lng cn, ly 25 ml dch nc trong cho tc dng vi 1 lng d (15 ln) thuc th Tris (1,10 - Phenaltrolin) cadimi (khong 10 ml). Lc k trong 10 pht, sau cho 5ml dung mi nitrobenzen v lc tip trong 30 pht. yn cho phn lp hon ton trong phu chit ri tch ly phn dung mi hu c cha phc lin hp ra. Tro ha t dung dch chit ny bng 30 ml axit nitric 65% v vi git hydropeoxyt 30% trong bnh keldan n khi thu c dung dch mu trong. Chuyn ton b mu ra cc chu nhit v c cn ui axit. Sau thm 5ml axit clohydric 1% vo cc, chuyn dung dch ny sang bnh nh mc v nh mc bng axit clohydric 1% n th tch 20 ml ri tin hnh xc nh cadimi. 5.2 Pha dy chun: Dng dung dch gc tiu chun ca cadimi nng 1 mg/ml v axit clohydric 1% pha long. Tnh lng ph hp pha dy chun c nng ca cadimi l 0, 1 - 0,5 - 1,0 - 1,5 - 2,0 - 2,5 g/ml trong bnh nh mc c th tch 25 ml 5.3 Chun b mu trng: ng thi vi vic chun b mu phn tch phi chun b thm mu trng so snh v b chnh nn. Mu trng c chun b nh mu phn tch nhng khng c mu phn tch. 5.4 Cc iu kin thc nghim: + Vch ph o ca cadimi 228,8nm; + Khe o my AAS 0,5 nm + Burner: Loi khe di 10 cm + Cng n catt rng : dng 80% gi tr cc i + Hn hp kh: khng kh nn v axetylen 4,2/1,2 lt/ pht + Tc dn mu : 4, 5 - 5 ml / pht + Thi gian o: 5 - 10 giy + Cc iu kin khc chn ph hp vi my AAS 6 Tin hnh th + t cc thng s chn mc 5.4 cho my o cadimi + Cho my chy n nh (15 pht) + o ph hp th ca cadimi ln lt t cc mu chun, mu trng. Ri n mu phn tch. Mi mu o 3 ln ly gi tr l trung bnh cng ca 3 ln th ng thi c sai lch gi tr khng vt qu 15%. + Hiu chnh gi tr ca mu trng (nu c) + Dng ng chun theo h ta D -C. Trong D l cng ca vch ph hp th ca cadimi trong cc mu chun tng ng vi cc nng C ca n trong dy chun. + Xc nh nng Cx ca cadimi trong mu phn tch theo ng chun trn. 7 Tnh kt qu Tng hm lng ca cadimi trong mu phn tch c tnh theo cng thc sau C - Cx .V y V = 20 ml v C tnh bng Mg Sau khi xc nh c hm lng cadimi trong mu phn tch ta suy ra lng penicillin theo phn ng sau: Penicillin + Tris ( 1,10 - phenal trolin) Cd phc lin hp Cd( phenaltrolin)3(Penicillin)2 Theo thnh phn ca phc lin hp ta thy rng:

1 nguyn t cadimi tng ng vi 2 phn t penicillin hay 112,4 g cadimi tng ng vi 2 mol penicillin hay 112,4 g cadimi tng ng vi 2 mol penicillin Vy 1 g cadimi tng ng vi 2/112,4 mol penicillin. Do Cg 2.C/112,4 mol G = 2.C/112,4.a Tnh bng mol/g Ch thch Nu sau khi chit phc bng nitrobenzen m tin hnh o ngay cadimi trong phc th mu chun cng phi chit bng nitrobenzen ri mi o. y cn lu v thuc th Tris (1,10 - Phenaltrolin) Cd ly d 15 ln nn dy dung dch chun khng phi l dung dch cadimi gc m l dung dch penicillin gc. Sau cho lng dung dch gc ny tc dng vi lng d thuc th, sau chit bng nitrobenzen ri mi o v xc nh trc tip tng penicillin trong mu theo dy dung dch chun. Cch ny phc tp v tn mt lng ln dung mi nn ta phi tin hnh v c ha tip ( nh mc 5.1). Theo phng php ny th dung dch chun gc l dung dch cha ion Cd2+. Suy ra cng thc tnh hm lng tng penicillin l

PH LC
1. Pha dung dch gc tiu chun ca cadimi nng 1mg/ml; cn 1,1423g cadimi oxyt bt (Cd0), thm 40 ml axit nitric 6M, un nh cho tan ht, ngui ri nh mc bng nc ct n 1 lt. Dung dch ny gi l dung dch A. 2. Dung dch cadimi nng 10g/ml; ly 1 ml dung dch A, pha long v nh mc bng axit nitri 1% n 100ml. Dung dch ny gi l dung dch B. 3. Dung dch cadimi nng 0,1 g/ml: ly 1 ml dung dch B, pha long v nh mc bng axit nitric 1% n th tch 100ml.