一步式QuEChERS结合超高效液相色谱-质谱法检测豇豆和芒果中22种农药残留
Determination of 22 Pesticide Residues in Cowpeas and Mangoes by One-step QuEChERS Combined with Ultra Performance Liquid Chromatography-Mass Spectrometry
仝凯旋 1夏寒 1李建勋 2谢瑜杰 1吴兴强 1范春林 1陈辉1
作者信息
- 1. 中国检验检疫科学研究院,北京 100176
- 2. 中国农业科学院农产品加工研究所,北京 100193
- 折叠
摘要
基于超高效液相色谱-串联质谱法(UPLC-MS/MS)建立了 豇豆和芒果中22种农药的一步式QuEChERS自动化检测技术,样品经1％乙酸乙腈提取,加入EN萃取盐(无水硫酸镁、氯化钠、柠檬酸三钠、柠檬酸二钠)除水后,使用C18和石墨化碳黑(GCB)净化,经ACQUITY UPLC BEH C18色谱柱分离,以0.01％甲酸水溶液(含2mmol/L甲酸铵)-0.01％甲酸甲醇为流动相,在多重反应监测(MRM)下进行测定.结果表明,22种农药在0.01～25.00 μg/L质量浓度范围内线性关系良好,决定系数R2均大于0.994,方法的检出限(LOD,S/N=3)在0.05～2 μg/kg范围内,定量限(LOQ,S/N=10)在0.1～5 μg/kg范围内,在1倍LOQ、2倍LOQ和10倍LOQ 3个加标水平下进行回收率实验(n=6),豇豆3个水平的平均回收率分别为70.9％～116.6％、71.9％～118.3％、73.7％～113.7％,芒果平均回收率分别为70.2％～114.6％、71.2％～113.7％、74.3％～118.5％,两种基质相对标准偏差均在20％以内.方法成功应用于42批实际样品检测,有33批检出农药残留.该方法有较高的灵敏度和足够自动化,减少了人为操作步骤,适用于22种农药及农药代谢物的同时检测及准确定量.
Abstract
A one-step QuEChERS automated detection technology for 22 pesticides in cowpeas and mangoes was established based on ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted by acetonitrile containing 1％acetic acid,added with EN extraction salt(anhydrous Mg2SO4,sodium chloride,trisodium citrate dihydrate,disodium hydrogen citrate sesquihydrate)to remove water,and then purified with C18 and graphitized carbon black(GCB).The target analytes were separated by ACQUITY UPLC BEH C18 chromatography column,using 0.01％formic acid aqueous solution(containing 2 mmol/L ammonium formate)-0.01％formic acid methanol as the mobile phase,and determined in multiple reaction monitoring(MRM).The results showed that the 22 pesticides had good linearity in the range of 0.01～25.00 μg/L,with coefficient of determination(R2)higher than 0.994.The limits of detection(LOD,S/N=3)were 0.05～2 μg/kg,and the limits of quantification(LOQ,S/N=10)were 0.1～5 μg/kg.At the spiked levels of 1×LOQ,2×LOQ,and 10×LOQ,the average recoveries for cowpeas were 70.9％～1 16.6％,71.9％～118.3％,and 73.7％～113.7％,respectively,and for mangoes were 70.2％～114.6％,71.2％～113.7％,and 74.3％～118.5％,respectively.The relative standard deviations for them were all within 20％.The method was successfully applied to the detection of 42 actual samples,and 33 samples detected pesticide residues.This method has high sensitivity and a satisfactory level of automation,effectively reducing human operation steps.It is suitable for the simultaneous detection and accurate quantification of 22 pesticides and their metabolites.
关键词
一步式QuEChERS/超高效液相色谱-质谱法/农药残留/豇豆/芒果Key words
one-step QuEChERS/UPLC-MS/MS/pesticide residues/cowpea/mango引用本文复制引用
基金项目
中国检科院基本科研业务费项目(2022JK32)
国家市场监管重点实验室(热带果蔬质量与安全)基础应用研究课题资助项目(KF-2023004)
出版年
2024
国家科技期刊平台
NSTL
万方数据