TIU CHUN VIT NAM TCVN 8323 : 2010

RAU QU - XC NH D LNG FLUSILAZOLE - PHNG PHP SC K KH Vegetables and fruits - Determination of flusilazole residues - Gas chromatographic method Li ni u TCVN 8323:2010 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 FLUSILAZOLE - PHNG PHP SC K KH Vegetables and fruits - Determination of flusilazole 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 flusilazole 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 flusilazole trong mu th c chit bng dung mi axeton sau c xc nh bng thit b sc k kh vi detector nit-phospho (NPD). 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 qui nh khc. 4.1. Axeton, tinh khit phn tch. 4.2. Diclometan, tinh khit phn tch. 4.3. Ete du m, nhit si trong di t 40oC n 60oC. 4.4. Toluen, tinh khit phn tch. 4.5. Natri sulfat khan, hot ha 130oC trong 8 h, ngui trong bnh ht m, bo qun trong bnh kn. 4.6. Hn hp dung mi, cha n-hexan v toluen vi t l th tch 9:1. 4.7. Cht chun flusilazole, bit tinh khit. 4.8. Dung dch chun gc, nng 100 g/ml Dng cn phn tch (5.8) cn 0,01 g cht chun flusilazole (4.7), chnh xc n 0,01 mg, cho vo bnh nh mc dung tch 10 ml (5.1), thm toluen (4.4) n vch v trn. 4.9. Dung dch chun trung gian, nng 10 g/ml Dng micropipet (5.3) ly 200 l dung dch chun gc flusilazole (4.8) cho vo bnh nh mc dung dch 20 ml (5.1), thm hn hp dung mi (4.6) n vch v trn.

4.10. Dung dch chun lm vic Pha long lin tc dung dch chun trung gian (4.9) thu c 3 dung dch chun lm vic vi cc nng tng ng l 1 g/ml (dung dch chun lm vic 1), 0,5 g/ml (dung dch chun lm vic 2) v 0,05 g/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. 4.11. Kh heli, c tinh khit khng nh hn 99,999 %. 4.12. Kh hydro, c tinh khit khng nh hn 99,999 %. 4.13. Khng kh nn dng cho thit b st k kh. 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 10 ml v 20 ml. 5.2. Pipet, dung tch 1 ml v 2 ml. 5.3. Micropipet, c th o t 50 l n 200 l 5.4. Cc ly tm, dung tch 250 ml hoc loi tng ng. 5.5. Bnh nn, dung tch 100 ml. 5.6. Xyranh, dung tch 10 l, chia vch n 1 l. 5.7. ng ong, dung tch 50 ml. 5.8. Cn phn tch, c th chnh xc n 0,01 mg. 5.9. Cn k thut, c th cn chnh xc n 0,01 g. 5.10. Thit b ng ha Ultra-Turrax, tc khng nh hn 13 500 r/min. 5.11. Thit b c quay chn khng 5.12. My nghin mu. 5.13. My ly tm, tc khng nh hn 2 000 r/min, c ng ly tm dung tch 250 ml. 5.14. Thit b sc k kh, c trang b nh sau: - bung bm mu, chia dng v khng chia dng: - detector nit - phospho (NPD); - ct mao qun DB-5, di 30 m, ng knh 0,32 mm, chiu dy pha tnh 0,25 m, 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 (5.12) n khi ng nht.

7.3. Chun b phn mu th Dng cn (5.9) cn khong 20 g mu th (m) c ng nht (xem 7.2), chnh xc n 0,01g, vo cc ly tm dung tch 250 ml (5.4). Thm vo cc 40 ml axeton, ng ha trong 30 s bng thit b Ultra-Turrax (5.10) vi tc 13 500 r/min, thm ln lt 40 ml ete du m, 40 ml diclometan, 5g natri sulfat khan, ng ha trong 30 s bng thit b Ultra-Turrax (5.10) vi tc 13 500 r/min, sau ly tm bng thit b ly tm (5.13) vi tc 2 000 r/min trong 10 min, thu ton b dch chit v ghi li th tch (V1). Dng ng ong (5.7) ly 30 ml (V2) dch lng thu c cho vo bnh nn dung tch 100 ml (5.5) v c cn (lm bay hi) bng thit b c quay chn khng (5.11) 40oC, dng 2 ml (VE) hn hp dung mi (4.6) ha tan d lng thu c phn mu th. 7.4. Chun b phn mu trng Mu trng l mu c bit trc khng cha d lng flusilazole, c chun b theo quy trnh trong 7.3. 7.5. Chun b phn mu kim tra hiu sut thu hi Dng cn (5.9) cn khong 20 g mu trng c ng nht (xem 7.2), chnh xc n 0,01 g, vo cc ly tm dung tch 250 ml (5.4). Dng micropipet (5.3) thm 200 l dung dch chun trung gian (4.9), 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; 2 l, khng chia dng; nhit ban u 80oC gi trong 1 min, tng 40oC/min n nhit 160oC, tng 3oC/min n 250oC, tng 10oC/min n nhit cui 280oC v gi trong 10 min; 1,7 ml/min; 270oC; 4 ml/min; 120 ml/min; 10 ml/min.

Tc kh mang (He): Nhit detector: Tc kh hydro (H2): Tc dng khng kh: Tc kh heli b tr: 7.7. Dng ng chun

Dng ng chun ca flusilazole (tng quan gia din tch/chiu cao pc 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 (4.10). 7.8. Xc nh Bm ln lt dung dch phn mu trng (7.4), dung dch phn mu th (7.3), dung dch phn mu kim tra hiu sut thu hi (7.5) vo thit b sc k kh (5.14). Xc nh nng 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 flusilazole, X, biu th bng miligam trn kilogam (mg/kg), c tnh theo cng thc:

X = X0
trong :

VE V1 P V2 m 100

X0 l nng flusilazole c xc nh bng ng chun (7.8), tnh bng microgam trn mililit (g/ml); VE l th tch mu th (xem 7.3), tnh bng mililit (ml); V1 l th tch dch chit thu c (xem 7.3), tnh bng mililit (ml); V2 l th tch dch chit c ly ra lm bay hi (xem 7.3), 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 (%). 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): 0,02 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] Food and Drug Aministration of USA, 1994, Pesticide Analysis Manual, Volume 1, Section 302, E1.