氧化石墨烯注射式净化结合液质联用法检测菠菜中氨基甲酸酯类农药残留  

Determination of residues of carbamate pesticides in spinach bygraphene oxide injection purification combined with liquidchromatography-mass spectrometry

作　　者：倪永付 刘彤 王勇 刘慧 NI Yongfu;LIU Tong;WANG Yong;LIU Hui(Comprehensive Technical Service Center of Jining Customs,Jining 272000,Shandong,China)

机构地区：[1]济宁海关综合技术服务中心,山东济宁272000

出　　处：《农药》2023年第11期823-827,共5页Agrochemicals

基　　金：济宁市重点研发计划(2021ZDZP024)。

摘　　要：[目的]以氧化石墨烯为净化剂,建立注射式净化结合液质联用技术检测菠菜中8种氨基甲酸酯类农药残留的方法。[方法]样品经乙腈提取、注射式净化后,采用Poroshell 120 EC-C18色谱柱,以甲醇-0.1%甲酸水为流动相进行梯度洗脱分离,在多反应监测模式下进行质谱检测,采用空白基质标准曲线进行外标法定量。[结果]在优化的试验条件下,8种氨基甲酸酯类农药在5~300μg/L质量浓度范围内具有良好的线性关系,相关系数0.9801~0.9975,方法检出限0.02~0.58μg/kg,定量限0.06~1.95μg/kg。以空白菠菜样品为基质进行了1、2、5μg/kg 3个梯度添加量的加标回收试验,回收率为80.5%~105.2%,相对标准偏差(RSD)为1.12%~9.79%。[结论]该方法准确度高,高效快速,可用于菠菜中氨基甲酸酯类农药残留的快速检测。[Aims]Using graphene oxide as purifying agents,a method for the determination of residues of 8 carbamate pesticides in spinach by injection purification combined with liquid chromatography-mass spectrometry was established.[Methods]After being extracted with acetonitrile and purified by injection,the sample was subjected to Poroshell 120 EC-C18 chromatography column,using methanol-0.1%formic acid water as the mobile phase for gradient elution separation,mass spectrometry detection was performed in a multi reaction monitoring mode,and external standard quantification was used by a blank matrix standard curve.[Results]The results showed that under the optimized experimental conditions,good linear relationships were obtained for 8 carbamate pesticides in the concentration range of 5-300μg/L,with correlation coefficient of 0.9801-0.9975,LOD of 0.02-0.58μg/kg,and LOQ of 0.06-1.95μg/kg for the method.The spiked recovery test for blank spinach sample with 3 levels of 1,2,5μg/kg showed a recovery rate of 80.5%-105.2%,with relative standard deviation(RSD)of 1.12%-9.79%.[Conclusions]The method is accurate,efficient and rapid,and is suitable for the rapid detection of residues of carbamate pesticides in spinach.

关 键 词：氧化石墨烯 注射式净化 液质联用 氨基甲酸酯类农药 残留 

分 类 号：TQ450.2[化学工程—农药化工]