快速滤过型净化-液相色谱-串联质谱法测定豇豆中9种杀虫剂类农药残留  

Determination of 9 Insecticides Residues in Cowpea by Multi-Plug Filtration Cleanup with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：黄勇平 邓英林 万娜 宋禹 黄金妮 陈丽君 HUANG Yongping;DENG Yinglin;WAN Na;SONG Yu;HUANG Jinni;CHEN Lijun(Institute of Food Testing,Hainan Academy of Inspection and Testing,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety,State Administration for Market Regulation,Haikou 570314,China;Plant Protection Station of Hainan Provice,Haikou 571199,China)

机构地区：[1]海南省检验检测研究院食品检验检测中心,国家市场监督管理总局重点实验室(热带果蔬质量与安全),海南海口570314 [2]海南省植物保护总站,海南海口571199

出　　处：《食品安全导刊》2025年第12期67-72,共6页China Food Safety Magazine

基　　金：国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(No.ZZ-2023002,No.ZZ-2024026)。

摘　　要：建立了快速滤过型净化(multi-Plug Filtration Cleanup,m-PFC)结合液相色谱-串联质谱技术同时测定豇豆中氟苯虫酰胺等9种杀虫剂残留量的分析方法。豇豆样品经乙腈提取,加入柠檬酸缓冲盐分离有机相与水相,经过m-PFC净化,采用2 mmol·L^(-1)乙酸铵溶液-甲醇作为流动相,梯度洗脱,HSS T3色谱柱分离,在多反应监测模式下,采用基质匹配外标法定量。结果表明,在2~200μg·L^(-1),9种农药的线性关系良好,相关系数R~2均大于0.996,在0.01、0.02、0.10 mg·kg~(-1) 3个添加水平下,回收率为79.6%~98.4%,相对标准偏差为1.2%~11.0%。该方法前处理简单、快捷,准确度好,适用于批量豇豆样品中9种杀虫剂的测定。A method was developed for the simultaneous determination of nine insecticide residues in cowpea,including flubeniliprole,by liquid chromatography-tandem mass spectrometry(m-PFC).The cowpea samples were extracted by acetonitrile,the organic phase and the aqueous phase were separated by the addition of citric acid buffer salt,and purified by m-PFC,and 2 mmol·L-1 ammonium acetate solution-methanol was used as the mobile phase,gradient elution,HSS T3 column separation,and quantification using matrix-matched external standards in multireaction monitoring mode.The results showed that the linear relationship between the nine pesticides was good at 2~200μg·L^(-1),the correlation coefficient R2 was greater than 0.996,and the recovery rate was 79.6%~98.4%and the relative standard deviation was 1.2%~11.0%at the three addition levels of 0.01 mg·kg-1,0.02 mg·kg^(-1),0.10 mg·kg^(-1).The method was simple,fast and accurate,and was suitable for the determination of 9 pesticides in batch cowpea samples.

关 键 词：豇豆 杀虫剂 快速滤过型净化 液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学]