凝胶渗透色谱净化/气相色谱-串联质谱法同时测定大豆中23种酰胺类除草剂残留量  

Simultaneous Detection of 23 Amide Herbicides Residues in Soybean by Gas Chromatography Tandem Mass Spectrometry

作　　者：杨晓凤[1,2] 洪雪华 陈敏[1,2] 张宪[4] YANG Xiao-feng;HONG Xue-hua;CHEN Min;ZHANG Xian(Sichuan Academy of Agricultural Sciences Analysis and Testing Center,,Chengdu 610066,China;Sichuan Academy of Agricultural Sciences,Institute of Agricultural Quality Standard&Testing Technology,Chengdu 610066,China;Sichuan Jie Cheng Environment Technology Co.,Ltd.,Chengdu 610037,China;China Green Food Development Center,Beijing 100081,China)

机构地区：[1]四川省农业科学院分析测试中心,成都610066 [2]四川省农业科学院农业质量标准与检测技术研究所,成都610066 [3]四川洁承环境科技有限公司,成都610037 [4]中国绿色食品发展中心,北京100081

出　　处：《农药》2021年第3期207-210,共4页Agrochemicals

基　　金：西藏自治区科技攻关计划重点项目(XZ201801NB07);四川省农业科学院青年领军人才研究基金项目(2020LJRC015)。

摘　　要：[目的]建立一种同时测定大豆中23种酰胺类除草剂残留量的分析方法。[方法]采用乙腈提取目标物,结合凝胶渗透色谱净化方法,通过气相色谱-串联质谱多反应监测模式,采用基质匹配外标法定量。[结果]在0.0050~0.50 mg/L范围内,黄豆和黑豆基质中23种酰胺类除草剂的质量浓度与对应的峰面积成良好的线性关系。在0.010、0.10、1.00 mg/kg添加水平下,2种基质23种酰胺类除草剂残留的回收率为81.6%~113.0%,相对标准偏差(RSD)为3.1%~8.1%,方法定量限(LOQ)均为0.010 mg/kg。[结论]该方法简便、准确可靠,可为23种酰胺类除草剂残留的准确定性及定量提供参考依据。[Aims] This study aims to establish a method for simultaneous determination of 23 amide herbicides residues in soybean by the MRM mode of gas chromatography-tandem mass spectrometry(GC-MS/MS). [Me thods] The soybean and black beans samples were extracted with acetonitrile and purified with gel permeation chromatography(GPC). The matrix-matched external standard calibration curves were used for quantitative analysis. [Results] The results showed that the linearity of 23 amide herbicides residues in the soybeans and black beans ranged from 0.0050-0.50 mg/L, with the linear correlation coefficients higher than 0.99. The average recoveries ranged from 81.6-113.0% in two matrices at three levels(0.010, 0.10 and 1.00 mg/kg) and the relative standard deviation(RSD) ranged from 3.1-8.1%. The limits of quantitation(LOQ) were 0.010 mg/kg. [Conclusions] This method is simple, accurate and reliable, and suitable for the accurate qualitative and quantitative determination of 23 amide herbicides residues.

关 键 词：酰胺类除草剂 气相色谱-串联质谱 凝胶渗透色谱 大豆 

分 类 号：TQ450.2[化学工程—农药化工]