QuEChERS前处理联合UPLC–MS/MS法检测花生中22种农药残留

Determination of 22 Pesticide Residues in Peanut by Qu ECh ERS–UPLC–MS/MS

建立了Qu ECh ERS(Quick,Easy,Cheap,Effective,Rugged,Safe)前处理联合UPLC–MS/MS法检测花生中22种农药残留的方法。样品用10 m L乙腈提取,以多壁碳纳米管、N-丙基乙二胺为吸附剂,对2 m L提取液进行净化,净化液稀释至2倍体积,以MRM扫描方式、正负离子模式同时分析。22种农药在10,20,50μg/kg 3个添加水平下,平均回收率为70.6%~121.2%,相对标准偏差小于10%(n=6);多菌灵、抗蚜威、扑草净在0.05~10μg/L,啶虫脒、氟虫腈砜、苯醚甲环唑、哒螨灵、嘧霉胺、嘧菌酯在0.5~20μg/L,烯酰吗啉、噻虫嗪、氟啶脲、灭幼脲、吡虫啉、甲维盐、除虫脲、氟虫腈、氟甲腈、氟虫腈亚砜、咪鲜胺、二甲戊灵在0.5~50μg/L之间,阿维菌素在0.5~100μg/L范围内线性良好,相关系数r2均大于0.995 0。22种农药的定量限在2μg/kg以下,远低于各待测农药最高残留限量标准(MRL)。该法适于花生中农药残留的同时快速检测。

QuEChERS–UPLC–MS/MS was proposed for determination of22pesticide residues in peanut.The samplewas extracted with10mL acetonitrile.2mL of the supernatant was taken and cleaned up with multi-walled carbon nanotubes(MWCNTs)and PSA.After being diluted to2times volume,the purified solution was determined by UPLC–MS/MS underthe mode of MRM.ESI was adopted in MS operated in the positive negative ion switch mode.Recovery rates at the threeconcentrations of10,20,50μg/kg ranged from70.6%to121.2%with RSDs less than10%(n=6).Linear relationshipsbetween values of peak area and mass concentration were found in the range of0.05–10μg/L for carbendazim,pirimicarb and prometryne,0.5–20μg/L for acetamiprid,fipronil-sulfone,difenocoazole,pyridaben,pyrimethanil andazoxystrobin,0.5–50μg/L for dimethomorph,thiamethoxam,chlorfluazuron,chlorbenzuron,imidacloprid,emamectinbenzoate,diflubenzuron,fipronil,fipronil-desulfinyl,fipronil-sulfide,prochloraz and pendimethalin,and0.5–100μg/Lfor abamectin,with the linear relative coefficients(r2)more than0.9950.The LOQs of22pesticide residues were less than2μg/kg,which were significantly lower than the respective MRLs.This method can be used in the determination of22pesticide residues in peanut.