QuEChERS-超高效液相色谱-串联质谱法检测中药砂仁中10种氨基甲酸酯类农药残留  

Determination of 10 Carbamate Pesticide Residues in Amomum villosum Lour.by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张振山[1] 乐渊[1] 黎舒怀[1] 刘春华[1] 李萍萍[1] ZHANG Zhen-shan;LE Yuan;LI Shu-huai(Analysis&Test Center,Chinese Academy of Tropical Agricultural Sciences,Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Haikou,Hainan 571101)

机构地区：[1]中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室,海南海口571101

出　　处：《安徽农业科学》2021年第1期199-202,206,共5页Journal of Anhui Agricultural Sciences

基　　金：中国热带农业科学院基本科研业务费专项资金(1630082020001,1630082020002)。

摘　　要：[目的]建立QuEChERS-超高效液相色谱-串联质谱检测砂仁中10种氨基甲酸酯类农药残留量的方法。[方法]砂仁样品先用含1%甲酸的乙腈溶液提取,再经盐析剂盐析后加入MgSO 4、PSA和C 18进行萃取、净化,采用UPLC-MS/MS检测,基质匹配标准曲线外标法进行定量。[结果]目标化合物在2.5~100.0μg/L有良好的线性关系,R 2≥0.999;在0.02、0.08和0.40 mg/kg 3个添加水平下,10种农药成分加标回收率为70.7%~113.3%,RSD为0.2%~4.9%(n=3);定量限(LQD)在0.19~4.01μg/kg。[结论]该方法操作简单、净化效果好、灵敏度高、准确度高,适用于砂仁药材中10种氨基甲酸酯类农药的残留检测。[Objective]To establish a method for the simultaneous determination of 10 carbamate pesticide residues in Amomum villosum Lour.by QuEChERS-ultraperformance liquid chromatography-tandem mass spectrometry.[Method]The samples were extracted with acetonitrile(containing 0.1%formic acid)and followed by salting-out process,the extract was further purified by C 18,PSA and anhydrous magnesium sulfate.The prepared samples were then analyzed by UPLC-MS/MS and quantified by the matrix-matched standard calibration curve method.[Result]The target compound had a good linear relationship between 2.5-100.0μg/L,R 2≥0.999;at spiked levels of 0.02,0.08 and 0.40 mg/kg,the average recoveries of all the pesticides were 70.7%-113.3%,and the RSD was 0.2%-4.9%(n=3).The limits of detection(LOD)was 0.19-4.01μg/kg.[Conclusion]The method has simple operation,good purification effect,high sensitivity and high accuracy,and is suitable for the detection of 10 carbamate pesticide residues in Amomum vilosum Lour..

关 键 词：砂仁 氨基甲酸酯类农药 QuEChERS-超高效液相色谱-串联质谱 

分 类 号：S481.8[农业科学—农药学]