QuEChERS高效液相色谱-串联质谱法测定水果中灭蝇胺、阿维菌素、涕灭威、涕灭威砜、涕灭威亚砜的残留量

Determination of cyromazine,avermectin,aldicarb,aldicarb-sulfone and aldicarb-sulfoxide residues in fruits by QuEChERS-HPLC-MS/MS

目的建立QuEChERS高效液相色谱-串联质谱法测定水果中灭蝇胺、阿维菌素、涕灭威、涕灭威砜、涕灭威亚砜等5种农药残留量的检测方法。方法样品以乙腈为提取液,经超声振荡提取后,加入QuEChERS萃取盐包,混匀离心。取上清液经QuEChERS小管净化后,高效液相色谱-串联质谱仪测定,采用正离子多反应监测(MRM)模式,外标法定量。结果在优化后的色谱和质谱条件下,5种农药浓度为1.0 ng/ml~100.0 ng/ml,线性关系良好,相关系数(r)≥0.9975,方法检出限≤0.3μg/kg,不同基质中平均加标回收率为82.2%-121.4%,相对标准偏差(RSD)为3.8%~13.6%。结论该方法样品前处理简单,分析效率高,净化效果好,操作时间短,可广泛适用于同时测定水果中灭蝇胺、阿维菌素、涕灭威、涕灭威砜、涕灭威亚砜等5种农药的残留量。

Objective To establish a QuEChERS high-performance liquid chromatography-tandem mass spectrometric method(HPLC-MS/MS)for the-simultaneous determination of 5 pesticides residues(cyromazine,avermectin,aldicarb,aldicarb-sulfone and aldicarb-sulfoxide)in fruits.Methods The sample was extracted with acetonitrile as the extraction solution by ultrasonic oscillation,then added with QuEChERS extraction salt package,mixed and centrifugated.The supernatant was purified by QuEChERS tubule,and then determined by high performance liquid chromatography-tandem mass spectrometer(HPLC-MS/MS).Positive ion multiple reaction monitoring(MRM).mode was adopted and quantified by external standard method.Results Under the conditions of optimized chromatography and mass spectrometric,the calibration curves for the 5 pesticides residues were linear in the range of 1.0 ng/ml-100.0 ng/ml with the correlation coefficient of(r)≥ 0.9975,and the detection limits were less than 0.3μg/kg.The average recovery rates of 5 pesticides residues from different matrices were within 82.2%-121.4%,with relative standard deviation(RSD)of 3.8%-13.6%.Conclusion The method is simple in operation,and of high sensitivity,better purification effect and rapid determination.It is suitable for the determination of the 5 pesticides residues(cyromazine,avennectin,aldicarb,aldicarb-sulfone and aldicarb-sulfoxide)in fruits.