高效液相色谱-串联质谱法测定9种农产品中41种农药残留量

Determination of 41 kinds of pesticide residues in 9 kinds of agricultural products by high performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)法检测9种农产品中41种农药残留的分析方法。方法前处理采用改进的QuEChERS方法,样品经乙腈提取、超声后,用QuEChERS法净化上清液,有效降低样品中复杂基质所带来的背景干扰,再经HPLC-MS/MS分析,外标定量。结果 41种农药残溜在1~50μg/L范围内具有较好的线性关系,相关系数均大于0.995,加标水平为5、15、30μg/kg时, 41种农药的回收率在70%~120%,相对标准偏差小于15%,9种农产品进行加标回收率为62.7%~115.5%。结论此方法适用于番茄、苹果等9种农产品中41种农药残留的检测。

Objective To establish a method for the determination of 41 kinds of pesticide residues in 9 kinds of agricultural products by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample was pre-processed by the improved QuEChERS method,extracted with acetonitrile,followed by ultrasonic extraction at lower temperatures.The supernatant was purified with QuEChERS method to effectively reduce the background interference caused by the complex matrix in the sample,and then analyzed by HP LC-MS/MS for external standard quantification.Results The 41 pesticides had good linear relationships in the range of 1.0-50μg/L,with correlation coefficients more than 0.995.The recoveries of the 41 pesticides at 3 spiked levels(5,15,30μg/kg)were 70%-120%,with the relative standard deviations were less than 15%.The standard recovery rates of 9 kinds of agricultural products were 62.7%-115.5%.Conclusion This method is applicable for the detection of 41 pesticide residues in 9 kinds of agricultural products such as tomatoes and apples.