QuEChERS-液质联用法同时测定农产品中3种农药及其代谢物残留

Simultaneous Determination of Three Pesticides and Their Metabolite Residues in Agricultural Products by-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

[目的]建立同时检测农产品中甲拌磷、丙硫菌唑和氟虫腈及其代谢物残留的QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)方法。[方法]样品用乙腈提取,经C 18 净化,采用UPLC-MS/MS检测,基质匹配外标法进行定量。[结果]在5种基质(糙米、面粉、玉米、白菜、苹果)中,农药及代谢物在0.005~0.500 mg/L线性关系良好,相关系数大于0.996,定量限均小于10 μg/kg。在0.01、 0.10 和1.00 mg/kg添加水平下,平均回收率为71.2%~105.0%,相对标准偏差(RSD)为1.28%~16.70%。[结论]该方法灵敏度、准确度和精密度均满足农药残留分析的要求,可用于农产品中甲拌磷、丙硫菌唑和氟虫腈及其代谢物残留的同时检测。

[Objective]The research aimed to establish a method of simultaneous detection of phorate,prothioconazole and fipronil and its metabolite residues in agricultural products by QuEChERS-UPLC-MS/MS.[Method]The samples were extracted with acetonitrile,and cleaned up by C 18 ,determined by UPLC-MS/MS and quantified by the matrix-matched external standard method.[Result]The calibration curves were linear in the range of 0.005-0.500 mg/L with the correlation coefficients larger than 0.996,the limits of quantitation were less than 10 μg/kg in five different matrix (brown rice,wheat flour,maize,Chinese cabbage,apple).The mean recovery of 9 pesticides were 71.2%-105.0% and the relative standard deviation (RSD) was 1.28%-16.70% at 0.01,0.10 and 1.00 mg/kg with hree spiked levels.[Conclusion]The sensitivity,accuracy and precision of the method meet the requirements of pesticide residue analysis,and can be used for simultaneous detection of phorate,prothioconazole and fipronil and their metabolite residues in agricultural products.