亲脂性匹配色谱分离-超高效液相色谱-串联质谱法测定果蔬中21种三唑类杀菌剂
Determination of 21 Triazole Fungicides in Fruits and Vegetables by Lipophilicity-matched Chromatographic Separation-Ultra Performance Liquid Chromatography-tandem Mass Spectrometry
孟虎 1李源槿 2赵丹妮 1张雅婷 1张丹 1杨琦 1冯歆轶1
作者信息
- 1. 西安市产品质量监督检验院,陕西西安 710065
- 2. 陕西中检评价技术有限公司,陕西西安 710065
- 折叠
摘要
为了提高农药残留的色谱分离效率和降低基质效应,本研究提出亲脂性匹配色谱分离,选取三唑类杀菌剂为研究对象,建立了果蔬中21种三唑类杀菌剂的超高效液相色谱-串联质谱(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法.样品经乙腈提取,盐析分相,分散固相萃取净化,选用与三唑类杀菌剂具有相近亲脂性的色谱柱进行分离,探究不同亲脂性烷基键合相对基质效应、回收率以及三唑杀菌剂和基质组分色谱分离的影响.结果表明,亲脂性匹配色谱分离能够提高色谱分离效率,改善三唑杀菌剂和基质组分的色谱分离,21种三唑杀菌剂的基质效应为-8.3%～4.7%,在 5～250 μg/L浓度范围内线性关系良好,决定系数R2≥0.999,平均回收率为 91.4%～108.1%,定量限为 0.5～3.5 μg/kg.该检测方法能够有效降低基质效应,使用溶剂校准曲线进行定量即可获得满意的回收率,显著提高了检测效率,具有简便、准确、灵敏度高等特点,适用于果蔬中三唑杀菌剂的检测.所述亲脂性匹配色谱分离,为农药残留的液相色谱-串联质谱法分析中液相色谱柱的选择和基质效应的降低提供了方法参考.
Abstract
In order to improve the chromatographic separation efficiency of pesticide residues and reduce matrix effects,a lipophilicity-matched chromatographic separation strategy was proposed in this study.The triazole fungicides in fruits and vegetables were selected as a case study to establish the analytical method of 21 triazole fungicides with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted by acetonitrile,followed by salting out and cleaned-up with dispersive solid phase extraction,then separated on chromatographic column with similar lipophilicity to triazole fungicides.The effects of alkyl bonded phase with different lipophilicity on the matrix effects,recoveries and chromatographic separation of triazole fungicides and matrix components were explored.The results showed that this strategy could improve the chromatographic separation of triazole fungicides and matrix components.And 21 triazole fungicides had matrix effects within-8.3%～4.7%and good linear relationship within 5～250 μg/L,the determination coefficient R2≥0.999.The average recoveries ranged from 91.4%to 108.1%,while the limits of quantitation were in the range of 0.5～3.5 μg/kg.This method could effectively reduce matrix effects and provide satisfactory recoveries using solvent calibration for quantification,which could significantly improve the detection efficiency.The proposed method was simple,accurate and sensitive,and suitable for determination of triazole fungicides in fruits and vegetables.This strategy could provide a method reference for column selection and matrix effect reduction in liquid chromatography-tandem mass spectrometry analysis.
关键词
亲脂性匹配色谱分离/基质效应/三唑类杀菌剂/分散固相萃取/超高效液相色谱-串联质谱Key words
lipophilicity-matched chromatographic separation/matrix effect/triazole fungicides/dispersive solid-phase extraction/ultra performance liquid chromatography-tandem mass spectrometry引用本文复制引用
基金项目
陕西省市场监督管理局科技计划项目(2020KY09)
出版年
2024
国家科技期刊平台
NSTL
维普
万方数据