TIU CHUN VIT NAM TCVN 8322 : 2010

RAU QU - XC NH D LNG 2,4-D PHNG PHP SC K KH Vegetables and fruits Determination of 2,4-D residues Gas chromatographic method Li ni u TCVN 8322 : 2010 do Cc Bo v thc vt bin son, B Nng nghip v Pht trin nng thn ngh, Tng cc Tiu chun o lng Cht lng thm nh, B Khoa hc v Cng ngh cng b. RAU QU - XC NH D LNG 2,4-D PHNG PHP SC K KH Vegetables and fruits Determination of 2,4-D residues Gas chromatographic method 1. Phm vi p dng Tiu chun ny quy nh phng php xc nh d lng thuc bo v thc vt 2,4-D trong rau v qu bng sc k kh. 2. Ti liu vin dn Cc ti liu vin dn sau rt cn thit cho vic p dng tiu chun ny. i vi cc ti liu vin dn ghi nm cng b th p dng phin bn c nu. i vi cc ti liu vin dn khng ghi nm cng b th p dng phin bn mi nht, bao gm c cc sa i, b sung (nu c). TCVN 4851 (ISO 3696), Nc dng phn tch trong phng th nghim Yu cu k thut v phng php th. 3. Nguyn tc D lng 2,4-D trong mu th c chit bng dung mi metanol, c este ho v c xc nh bng thit b sc k kh vi detector cng kt in t (ECD). 4. Thuc th Ch s dng cc thuc th loi tinh khit phn tch, nc loi 3 ca TCVN 4851 (ISO 3696), tr khi c quy nh khc. 4.1. Diclomotan 4.2. n-hexan 4.3. Axit sulfuric m c 4.4. Natri sulfat khan, hot ho 130oC trong 8h, ngui trong bnh ht m, bo qun trong bnh kn. 4.5. Celite 545 4.6. Giy ch th pH 4.7. Dung dch H2SO4, nng 3M 4.8. Dung dch NaOH, nng 5M 4.9. Dung dch NaHCO3 Cn 4g NaHCO3 vo bnh nn dung tch 100ml, thm nc n vch v trn 4.10. Hn hp dung mi 1, cha nc ct v metanol vi t l th tch 2 : 8 4.11. Hn hp dung mi 2, cha axit sulfuric m c v metanol vi t l th tch 1 : 9 4.12. Cht chun 2,4-D v 2,4-D metyl este, bit tinh khit.

4.13. Dung dch chun gc, nng 1000 g/ml Dng cn phn tch (5.10) cn 0,01g tng cht chun 2,4-D v 2,4-D metyl este (4.12), chnh xc n 0,01 mg, cho vo cc bnh nh mc dung tch 10ml (5.1), thm n-hexan n vch v trn. 4.14. Dung dch chun trung gian, nng 10 g/ml Dng micropipet (5.3) ly 200 l dung dch chun gc 2,4-D metyl este (4.13) cho vo bnh nh mc dung tch 20ml (5.1), thm n-hexan n vch v trn. 4.15. Dung dch chun kim tra hiu sut thu hi, nng 10g/ml Dng micropipet (5.3) ly 200 l dung dch chun gc 2,4-D (4.13) cho vo bnh nh mc dung tch 20ml (5.1), thm n-hexan n vch v trn. 4.16. Dung dch chun lm vic Pha long lin tc dung dch chun trung gian (4.14) thu c 3 dung dch chun lm vic vi cc nng tng ng l 1g/ml (dung dch chun lm vic 1), 0,5g/ml (dung dch chun lm vic 2) v 0,05g/ml (dung dch chun lm vic 3) Cc dung dch chun lm vic c bo qun 4oC v c thi hn s dng l 6 thng. 4.17. Kh nit, c tinh khit khng nh hn 99,999% 5. Thit b, dng c S dng cc thit b, dng c ca phng th nghim nh sau: 5.1. Bnh nh mc, dung tch 10ml v 20ml 5.2. Pipet, dung tch 1ml, 2ml v 5ml 5.3. Micropipet, dung tch t 50l n 200l 5.4. Cc ly tm, dung tch 250ml hoc loi tng ng. 5.5. Bnh cu, dung tch 100ml 5.6. Bnh nn, dung tch 100ml v 500ml 5.7. Phu chit, dung tch 100ml v 250ml 5.8. Xylanh, dung tch 10l, chia vch n 1l 5.9. ng ong, dung tch 25ml 5.10. Cn phn tch, c th cn chnh xc n 0,01mg 5.11. Cn, c th cn chnh xc n 0,01g 5.12. B phu lc Buchner 5.13. Thit b ng ho Ultra-Turrax, tc khng nh hn 13 500 r/min 5.14. Thit b c quay chn khng 5.15. My nghin mu 5.16. My ly tm, tc khng nh hn 2000 r/min, ng ly tm dung tch 250ml 5.17. Thit b sc k kh, c trang b nh sau: - bung bm mu, chia dng v khng chia dng; - detector cng kt in t (ECD) - ct mao qun DB-5, c chiu di 30m ng knh 0,32 mm, chiu dy pha tnh 0,25l, hoc loi tng ng;

- my vi tnh 6. Ly mu Vic ly mu khng c quy nh trong tiu chun ny. Nn ly mu theo TCVN 5139 : 2008 (CAC/GL 33-1999) Phng php khuyn co ly mu xc nh d lng thuc bo v thc vt ph hp vi cc gii hn d lng ti a (MRL) 7. Cch tin hnh 7.1. Yu cu chung Ton b qu trnh phn tch nn c thc hin trong ngy. Nu khng phn tch c trong ngy th phi bo qun dch mu 4oC. 7.2. Chun b mu Mu th c nghin trong my nghin mu (5.15) n khi ng nht 7.3. Chun b phn mu th 7.3.1. Chit tch Dng cn (5.11) cn khong 50g (m) mu th c ng nht (xem 7.2), chnh xc n 0,01g, vo cc ly tm dung tch 250ml (5.4). Thm vo cc 100ml hn hp dung mi 1 (4.10) v 5g celite (4.5), ng ho trong 30s bng thit b Ultra-Turrax (5.13) vi tc 13 500 r/min, sau lc bng b lc Buchner (5.12), trng ra bng 30ml hn hp dung mi 1 (4.10). Chuyn ton b dch lc vo bnh nn dung tch 500ml (5.6), dng pipet (5.2) thm 1ml dung dch NaOH 5M (4.8), kim tra v iu chnh pH khong 10. C cn (lm bay hi) ton b metanol bng thit b c quay chn khng (5.14) 40oC, thu c dung dch A. 7.3.2. Lm sch Chuyn ton b dung dch A vo phu chit dung tch 250ml (5.7), dng 50ml nc ct trng ra. Chit hai ln, mi ln bng 25ml diclometan (4.1), loi b pha hu c (pha di). Dng pipet (5.2) thm 5ml dung dch H2SO4 3M (4.7), kim tra v iu chnh pH khong 2. Chit 3 ln, mi ln bng 25ml diclometan (4.1), thu pha hu c (pha di) vo bnh cu dung tch 100ml (5.5), loi b nc bng natri sulfat khan (4.4). C cn (lm bay hi) bng thit b c quay chn khng (5.14) 40oC. 7.3.3. Este ho Dng pipet (5.2) cho 5ml hn hp dung mi 2 (4.11) vo bnh cu (xem 7.3.2), yn 10 min nhit phng, thnh thong lc nh. Chuyn dch c este ho vo phu chit dung tch 100ml (5.7), dng 15ml nc ct trng ra. Chit 1 ln bng 10ml (VE) n-hexan, loi b pha nc (pha di). Ra pha hu c bng 15ml dung dch NaHCO3 (4.9). Dng pipet (5.2) ly khong 2ml pha hu c (pha trn) thu c phn mu th. 7.4. Chun b phn mu trng Mu trng l mu c bit khng cha d lng 2,4-D v c chun b theo quy trnh trong 7.3 7.5. Chun b mu kim tra hiu sut thu hi Dng cn (5.11) cn khong 50g mu trng c ng nht (xem 7.2), chnh xc n 0,01g, vo cc ly tm dung tch 250ml (5.4). Dng micropipet (5.3) thm 100l dung dch chun kim tra hiu sut thu hi (4.16), yn trong nhit phng ti thiu 15 min. Tip tc thc hin theo 7.3. 7.6. iu kin phn tch Nhit bung bm mu: Th tch bm mu: Nhit ct tch: 240oC; 1l, khng chia dng; nhit ban u 80oC gi trong 1 min, sau tng dn vi tc

 tng 40oC/min n nhit 160oC, 3oC/min n 250oC, 10oC/min n nhit cui 280oC v gi trong 10 min; Tc kh mang (N2) Nhit detector Tc nit b tr 7.7. Dng ng chun Dng ng chun ca 2,4-D (tng quan gia din tch/chiu cao pic v nng cht chun) ti 3 im c nng tng ng trong dung dch chun lm vic 1, dung dch chun lm vic 2 v dung dch chun lm vic 3 (4.16). 7.8. Xc nh Bm ln lt dung dch mu trng (7.4), dung dch mu th (7.3), dung dch mu kim tra hiu sut thu hi (7.5) vo thit b sc k kh (5.17). Xc nh nng ca cc dung dch da vo ng chun. Nu nng ca mu th nm ngoi ng chun th iu chnh bng cch pha long dung dch phn mu th (khng pha long lng mu bm). 8. Tnh kt qu D lng 2,4-D, X, biu th bng miligam trn kilogam (mg/kg), c tnh theo cng thc: 2ml/min; 300oC; 60ml/min.

X = Xo
Trong :

VE P 0,94 m 100

Xo l nng 2,4-D c xc nh bng ng chun (xem 7.8), tnh bng microgam trn mililit (g/ml); VE l th tch n-hexan (xem 7.3.3), tnh bng mililit (ml); m l khi lng mu th, tnh bng gam (g); P l tinh khit ca cht chun, tnh bng phn trm (%); 0,94 l h s chuyn i t 2,4-D metyl este sang 2,4-D. 9. Hiu sut thu hi v gii hn xc nh 9.1. Hiu sut thu hi ca phng php: t 70% n 110%. 9.2. Gii hn nh lng ca phng php (LOQ): 0,01 mg/kg. 10. Bo co th nghim Bo co th nghim phi ghi r: a) mi thng tin cn thit v vic nhn bit y mu th; b) phng php ly mu s dng, nu bit; c) phng php th s dng v vin dn tiu chun ny; d) mi thao tc khng c quy nh trong tiu chun ny, hoc nhng iu c coi l t chn, v bt k chi tit no c nh hng n kt qu; e) kt qu th nghim thu c.

TH MC TI LIU THAM KHO

[1] British Crop Protection Council 2003, The Pesticide Manual.

[2] Federal Republic of Germany, 1992, Manual of Pesticide Residue Analysis, Volume II.