高效液相色谱-串联质谱法测定蔬菜中灭蝇胺残留量

Determination of Cyromazine Residues in Vegetables by High Performance Liquid Chromatography-Tandem Mass Spectrometry

本文开发和验证用于测定蔬菜中灭蝇胺残留量的高效液相色谱-串联质谱法。样品用乙腈-乙酸铵水溶液提取,经振荡提取后,采用QuEChERS净化包(PSA 150 mg,PestiCarb 15 mg,MgSO4900 mg)除杂净化,离心过膜,上机检测。待测样品净化液以流动相A(5 mmol·L^(-1)乙酸铵水溶液)、流动相B(乙腈)梯度洗脱,BEH C18色谱柱分离,正离子电喷雾(ESI+)电离,质谱多反应监测模式扫描分析,标准曲线(空白基质溶液配制系列标准曲线)外标法定量。灭蝇胺浓度在0~800μg·L^(-1)线性关系良好(r>0.999),在100μg·kg^(-1)、200μg·kg^(-1)、400μg·kg^(-1)3个标准物质添加水平下,灭蝇胺回收率在88.3%~94.0%,相对标准偏差为3.5%~5.2%,方法检出限、定量限分别为1.0μg·kg^(-1)和3.0μg·kg^(-1)。该检测方法能满足不同基质蔬菜中灭蝇胺残留量的测定需求。

This paper developed and verified a high performance liquid chromatography-tandem mass spectrometry method for the determination of cyromazine residues in vegetables.The samples were extracted with acetonitrileammonium acetate solution,and purified by QuEChERS purification package(PSA 150 mg,PestiCarb 15 mg,MgSO4900 mg)after vibration extraction,centrifuged through membrane,and tested on the computer.The purified liquid of the sample to be tested was gradient eluted with mobile phase A(5 mmol·L^(-1)ammonium acetate solution)and mobile phase B(acetonitrile),separated by BEH C18 column,ionized by positive ion electrospray(ESI+),scanned by mass spectrometry in multireaction monitoring mode,and quantified by external standard curve(blank matrix solution preparation series standard curve).The linearity of fenpropathrin concentration was good in 0~800μg·L^(-1)(r>0.999).With the addition of 100μg·kg^(-1),200μg·kg^(-1),and 400μg·kg^(-1)standard substances,the recovery rates of cyromazine were 88.3%~94.0%,and the relative standard deviations were 3.5%~5.2%.The detection limit and quantification limit of the method were 1.0μg·kg^(-1)and 3.0μg·kg^(-1),respectively.The detection method can meet the requirements of the determination of cyromazine residues in vegetables with different substrates.