超高效液相色谱-串联质谱法测定蔬菜和水果中腈吡螨酯残留量

Determination of Cyenopyrafen Residues in Fruits and Vegetables by UPLC-MS/MS

建立了蔬菜和水果中腈吡螨酯残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经乙腈均质提取,混合使用乙二胺-N-丙基硅烷(PSA)和C18两种基质分散净化剂净化,净化液过膜后直接进行UPLC-MS/MS检测。通过考察腈吡螨酯在不同果蔬样品中的基质效应发现,采用UPLC-MS/MS检测蔬菜和水果中腈吡螨酯残留量时,腈吡螨酯在不同种类样品中存在不同程度的基质减弱效应,采用空白基质溶液稀释标准建立校正的标准曲线外标法定量以消除基质效应。结果表明,腈吡螨酯在0.05~10μg/L浓度范围内具有良好的线性关系,相关系数不低于0.999 6。在0.000 05~2 mg/kg范围内进行加标回收率实验,平均回收率为81.1%~99.3%,相对标准偏差为4.7%~9.3%,方法的定量下限为0.043μg/kg,检出限为0.013μg/kg。

A method of ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS） was developed for the determination of cyenopyrafen residues in fruits and vegetables.The analytes were extracted from the samples using acetonitrile,and purified by dispersion solid phase extration using C18 and PSA as solid phase,then analyzed by UPLC-MS/MS.The matrix-induced weakening effect was observed in the analysis of cyenopyrafen by UPLC-MS/MS in serval samples including of cucumber,apple and onion.The interference of matrix was reduced by the matrix-matched calibration standards curve.The linear ranges of cyenopyrafen in different matrices ranged from 0.05μg/L to 10μg/L with correlation coefficients not less than 0.9996.The recoveries of cyenopyrafen in cucumber,grape,apple and scallion samples at spiked levels of 0.00005-2mg/kg were in the range of 81.1%-99.3%,with relative standard deviations（RSDs） of 4.7%-9.3%.The limit of quantitation was 0.043μg/kg and the limit of detection was 0.013μg/kg.