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QuEChERS-高效液相色谱-串联质谱法检测蔬菜中二硫代氨基甲酸酯(盐)残留量

Determination of Dithiocarbamate(Salt)Residues in Vegetables by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry
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摘要 文章建立了柱前衍生结合QuEChERS技术测定蔬菜中二硫代氨基甲酸酯(盐)类(Dithiocarbamates, DTCs)农药残留量的分析方法。蔬菜样品中的二硫代氨基甲酸酯(盐)类农药在碱性乙二胺四乙酸二钠溶液中转化为水溶性钠盐,经碘甲烷衍生后用QuEChERS技术提取和净化,以0.05%甲酸水溶液-乙腈作为流动相在C_(18)色谱柱上梯度洗脱与分离,在ESI+模式下采用多反应监测(Multiple reaction monitoring,MRM)测定,基质匹配标准曲线外标法定量。结果表明,二硫代氨基甲酸酯(盐)类农药在2.0-500μg/L之间具有良好的线性关系,相关系数均大于0.999。在普通白菜、茄子、黄瓜、豇豆、胡萝卜、韭菜6种不同类别的蔬菜中添加不同水平二硫代氨基甲酸酯(盐)类农药时,回收率范围在79.6%-109.5%,相对标准偏差为0.7%-10.9%。方法的检出限(以CS2计)为0.3-1.1μg/kg,定量限(以CS2计)为1.2-2.8μg/kg。该方法简便、快速、准确,可用于蔬菜中二硫代氨基甲酸酯(盐)类农药的残留确证检测。 A method for the determination of dithiocarbamates(DTCs)pesticide residues in vegetables using pre column derivatization combined with QuEChERS technology was established.The dithiocarbamate(salt)pesticides in vegetable samples are converted into water-soluble sodium salts in an alkaline disodium ethylenediaminetetra acetic acid solution.After derivatization with iodomethane,they are extracted and purified using QuEChERS technology.They are eluted and separated on a C_(18) chromatographic column using 0.05%formic acid aqueous solution-acetonitrile as a mobile phase.They are determined using multiple reaction monitoring(MRM)in the ESI*mode,and quantified using a matrix matching standard curve external standard method.The results showed that dithiocarbamate(salt)pesticides ranged from 2.0 to 500μg/L There is a good linear relationship between,with correlation coefficients greater than 0.999.When adding different levels of dithiocarbamate pesticides to different types of vegetables such as ordinary Chinese cabbage,eggplant,cucumber,cowpea,carrot,and leek,the recovery ranged from 79.6%to 109.5%,with an relative standard deviation of 0.7%to 10.9%.The detection limit(CS_(2))of the method is 0.3 to 1.1μg/kg,and the quantitative limit(CS_(2))is 1.2 to 2.8μg/kg.The method is simple,rapid,and accurate,and can be used for the determination of dithiocarbamate(salt)pesticide residues in vegetables.
作者 孟繁磊 张慧 谭莉 范宏 张惠峰 蔡红梅 宋志峰 MENG Fanlei;ZHANG Hui;TAN Li;FAN Hong;ZHANG Huifeng;CAI Hongmei;SONG Zhifeng(Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences,Changchun 130033,China;Jilin Provincial Key Laboratory of Agro-Environment and Agro-Products Safety,Changchun 130033,China)
出处 《食品科技》 CAS 北大核心 2023年第10期291-296,共6页 Food Science and Technology
基金 吉林省科技厅重点研发项目(20210202110NC) 吉林省农业科学院农业质量标准与检测技术研究所发展基金项目(ZBS20Q03)。
关键词 QUECHERS 蔬菜 二硫代氨基甲酸酯(盐)类农药 超高效液相色谱-串联质谱 QuEChERS vegetables dithiocarbamate(salt)pesticides ultra high performance liquid chromatography-tandem mass spectrometry
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