QuEChERS-高效液相色谱三重四级杆线性离子阱串联质谱法测定蔬菜中34种杀虫剂残留
Determination of 34 Insecticide Residues in Vegetables by QuEChERS-High-Performance Liquid Chromatography Triple Quadrupole Linear Ion Trap Tandem Mass Spectrometry
罗景阳 1李娇 1关健 2李巧莲 1王岩松 2袁帅1
作者信息
- 1. 沈阳市食品药品检验所,辽宁沈阳 110124
- 2. 辽宁省检验检测认证中心,辽宁沈阳 110036
- 折叠
摘要
本文通过QuEChERS净化方法结合高效液相色谱三重四级杆线性离子阱串联质谱建立蔬菜中34种杀虫剂的快速检测方法.样品通过乙腈(含1％乙酸)、1.5g醋酸钠、4g无水硫酸镁、1g氯化钠进行溶剂萃取,再通过 20 mg石墨化碳黑(GCB)、300 mg乙二胺-N-丙基硅烷化硅胶(PSA)、200 mg十八烷基硅烷键合硅胶(C18)和1000 mg无水硫酸镁净化处理,选择乙腈-水为流动相,采用多反应监测-信息依赖性获取-增强型子离子扫描(MRM-IDA-EPI)模式对样品进行检测,并建立EPI数据谱库.检测结果通过保留时间、离子对峰度比及数据库EPI谱图进行对比定性,采用基质匹配外标法定量.研究结果表明,以茄子、韭菜、豇豆、菠菜为基质代表,34种杀虫剂线性关系良好,R2≥0.99011,检出限为0.16～1.81 μg/kg,定量限为0.52～6.02 μg/kg,样品的加标回收率为73.51％～118.77％,精密度为0.01％～14.27％,并对蔬菜样品进行检测,噻虫胺检出率达58.23％.该方法具有检测快速有效、操作简便、数据准确、灵敏度高等特点,适合用于蔬菜中34种杀虫剂的检测.
Abstract
This article established a rapid detection method for 34 pesticides in vegetables by combining QuEChERS purification method with high-performance liquid chromatography triple quadrupole linear ion trap tandem mass spectrometry.The samples were extracted with acetonitrile(containing 1％acetic acid),1.5 g sodium acetate,4 g anhydrous magnesium sulfate,and 1 g sodium chloride.The extract was further purified using 20 mg graphitized carbon black(GCB),300 mg primary secondary amine(PSA),200 mg octadecylsilane chemically bonded silica(C18),and 1000 mg MgSO4.Acetonitrile-water was chosen as mobile phase.The samples were analyzed using MRM-IDA-EPI mode,and an EPI database was established.Qualitative analysis was performed based on retention time,ion pair peak ratio,and EPI database,and quantification was carried out using matrix-matched external standard method.The study results indicated that using eggplant,garlic chives,cowpea,and spinach as representative matrices,the 34 pesticides showed good linear correlation with R2≥ 0.99011.The detection limits ranged from 0.16 to 1.81 μg/kg,and the quantification limits ranged from 0.52 to 6.02 μg/kg.The spiked recoveries of the samples were between 73.51％and 118.77％,and the precision was in the range of 0.01％to 14.27％.Vegetable samples were tested,with a detection rate of 58.23％for thiamethoxam.This method was characterized by its rapid and effective detection,simple operation,accurate data,and high sensitivity,making it suitable for the detection of 34 pesticides in vegetables.
关键词
杀虫剂/高效液相色谱三重四级杆线性离子阱串联质谱/蔬菜/QuEChERSKey words
insecticide/high-performance liquid chromatography-triple quadrupole linear ion trap tandem mass spectrometry/vegetables/QuEChERS引用本文复制引用
基金项目
辽宁省市场监督管理局科技计划项目(2022ZC023)
沈阳市科技计划项目(22-322-3-37)
出版年
2024
国家科技期刊平台
NSTL
万方数据