超高效液相色谱-串联质谱法测定果蔬中胺苯吡菌酮残留量

Determination of fenpyrazamine residues in vegetables and fruits by UPLC-MS/MS

建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)法分析蔬菜和水果中胺苯吡菌酮残留量。用乙腈提取样品中残留的胺苯吡菌酮,提取液经十八烷基硅胶键合相(C_(18))和乙二胺-N-丙基硅烷(PSA)混合净化剂净化,使用UPLC-MS/MS电喷雾离子化、正离子扫描和多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。结果表明,胺苯吡菌酮在0.05~10μg/L范围线性关系良好,相关系数不低于0.9993。在0.1~2000μg/kg范围内,对黄瓜、菠菜、苹果、葡萄和洋葱样品进行添加回收率实验,平均回收率为81.2%~104.3%,相对标准偏差为2.2%~16%,方法的定量限为55 ng/kg,检出限为5.5 ng/kg。本研究建立的方法能对蔬果中胺苯吡菌酮残留量进行准确的定性和定量分析。

A determination method for fenpyrazamine residues in vegetables and fruits was established by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).The analytes were extracted from the samples using acetonitrile,and purified by dispersion solid phase extraction including C_(18)and primary secondary amine(PSA).Subsequently,the product was analyzed by UPLC-MS/MS with positive electrospray ionization under multiple reaction monitoring(MRM)mode.Meanwhile,matrix matching standard solution was quantified by external standard method.As the result,the linear range of fenpyrazamine in different matrices was0.05-10μg/L with the correlation coefficients of lower than 0.9993.The recoveries of fenpyrazamine from cucumber,leek,apple,grape and scallion samples at spiked levels of 0.1-2000μg/kg were in the range of81.2%-104.3%,and the relative standard deviations(RSDs)were 2.2%-16%.The limit of quantitation was 55 ng/kg,and the limit of detection was 5.5 ng/kg.This method is able to meet the requirements for the determination of fenpyrazamine residues in fruits and vegetables.