高效液相色谱-串联质谱法检测大豆和土壤中喹禾糠酯及代谢物的残留

Determination of Quizalofop-P-tefuryl and Metabolites Residue in Soybean and Soil by HPLC-MS/MS

利用高效液相色谱-串联质谱法检测大豆及土壤中喹禾糠酯和代谢物喹禾灵酸的残留及消解动态。样品用盐酸混合液和乙腈提取,石墨炭黑和C18填料净化,高效液相色谱串联质谱法检测,外标法定量。结果表明,喹禾糠酯及代谢物喹禾灵酸在大豆植株、籽粒、毛豆、土壤中的添加平均回收率分别为82.4%~95.3%、90.4%~101.9%,相对标准偏差分别为2.8%~10.3%、2.1%~10.9%。喹禾糠酯及代谢物喹禾灵酸在大豆籽粒上定量限为0.01mg/kg,在大立植株、毛豆和土壤中的定量限为0.005mg/kg;喹禾糠酯及代谢产物喹禾灵总量的消解半衰期在大豆植株上为7.0d,在土壤上为1.7d和2.0d,在毛豆和大豆中的最终残留量分别为<0.005mg/kg和<0.01 mg/kg。

The decline and final residue of quizalofop-P-tefuryl and quizalofop metabolites in soybean and soil was determined by HPLC-MS/MS.The sample was extracted with HC1 mixture and acetonitrile,purified by filling of graphite carbon black and Cl8,and quantified by external standard method.The result showed that the average recoveries of quizalofop-P-tefuryl and quizalofop metabolites in soybean plants and soil were 82.4%?95.3%and 90.4%?101.9%,respectively,that the standard deviation was 2.8%?10.3%and 2.1%?10.9%,respectively.The limit of quantification for quizalofop-P-tefuryl and quizalofop metabolites in soybean seed was 0.01 mg/kg and 0.005 mg/kg in soybean plants,green soybean and soil,respectively.The half-life was 7.Od in soybean plants and 1.7d?2.Od in soil.The final residual concentration was below 0.005 mg/kg in soybean and below 0.01 mg/kg in soil.