超高效液相色谱-串联质谱法测定蔬菜中4种氨基甲酸酯类农药残留量  

Determination of 4 kinds of carbamates pesticide in vegetables by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：陈俊秀[1] 马晓年[1] 李文廷[1] 梁志坚[1] 梁孟军[1] 张瑞雨[1] CHEN Jun-Xiu;MA Xiao-Nian;LI Wen-Ting;LIANG Zhi-Jian;LIANG Meng-Jun;ZHANG Rui-Yu(Kunming Center for Disease Control and Prevention,Kunming 650228,China)

机构地区：[1]昆明市疾病预防控制中心,昆明650228

出　　处：《食品安全质量检测学报》2021年第5期1789-1797,共9页Journal of Food Safety and Quality

基　　金：昆明市卫生科技人才培养项目暨“十百千”工程培养计划[2019-sw(后备)-50]。

摘　　要：目的建立超高效液相色谱-串联质谱法测定蔬菜中4种氨基甲酸酯类农药残留量。方法蔬菜样品经切碎,乙腈提取,分别用固相萃取柱及QuEChERS净化后,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,经CAPCELL PAK C_(18)色谱柱分离,采用多反应监测正离子模式(multireaction monitoring in positive ion mode,MRM)对异丙威、仲丁威、残杀威、克百威4种氨基甲酸酯类农药进行定性和定量分析。结果 4种氨基甲酸酯类农药在给定标准溶液浓度范围内峰面积与浓度呈良好线性关系,相关系数均大于0.999,检出限为0.001~0.005 mg/kg,平均回收率为70%~130%,相对标准偏差均小于20%。结论本方法灵敏度高、检出限低、回收率好、操作可行,可实现蔬菜中多种氨基甲酸酯类农药的同时测定。Objective To establish a method for the determination of 4 kinds of carbamates pesticide in vegetables by ultra performance liquid chromatography-tandem mass spectrometry.Methods Vegetable samples were chomped,extracted by acetonitrile,purified by solid phase extraction column and QuEChERS,respectively,eluted by acetonitrile-0.1%formic acid aqueous solution as mobile phase gradient,and separated by CAPCELL PAK C18 chromatographic column.Multireaction monitoring in positive ion mode(MRM)was used for qualitative and quantitative analysis for carbamate pesticides,isopropoxur,secobutycarb,and carboxycarb.Results The 4 kinds of carbamates in the range of a given standard solution concentration peak area and concentration had good linear relationship,the correlation coefficients were greater than 0.999,the limits of detection were 0.001‒0.005 mg/kg,the recoveries were 70%‒130%,and the relative standard deviations were less than 20%.Conclusion This method has the advantages of high sensitivity,low limit of detection,good recoveries,and feasible operation,which can realize multiple carbamates in vegetable products at the same time.

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

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]