基于QuEChERS-HPLC∕MRM-IDA-EPI技术测定茄子中11种农药残留  

Simultaneous determination of 11 pesticide residues in eggplant by QuEChERS-HPLC∕MRM-IDA-EPI method

作　　者：汤逸飞 屠雨晨 陈欣慰 黄芳 张国平 TANG Yifei;TU Yuchen;CHEN Xinwei;HUANG Fang;ZHANG Guoping(Jiaxing Center for Inspection and Testing of Agriculture,Jiaxing 314050,China)

机构地区：[1]嘉兴市农业综合检验检测中心,嘉兴314050

出　　处：《上海农业学报》2024年第3期92-100,共9页Acta Agriculturae Shanghai

基　　金：全国农产品质量安全检验检测体系建设项目[浙农计发(2015)7号];嘉兴市公益性研究计划项目(2021AY10082);桐乡市重点科技计划项目(202201062)。

摘　　要：利用乙腈溶液提取10.0 g茄子均质化样品,经乙二胺-N-丙基硅烷、石墨化炭黑、硫酸镁和氯化钠净化后利用快速前处理-高效液相∕多反应监测-信息依赖-增强型质谱扫描(QuEChERS-HPLC∕MRM-IDA-EPI)分析方法识别茄子中11种农药残留化合物的结构和合理的片段化离子,采用+MRM-IDA-EPI模式,外标法定量。结果显示:该方法在10—250μg∕L茄子加标基质内线性关系良好,回归方程相关系数(r)为0.9949—0.9999;在0.01—0.25 mg∕kg范围内添加回收率(P)为69.02%—127.49%,相对标准偏差(RSD)为1.48%—13.56%。可同时触发EPI模式,通过判断准分子离子峰、加钠离子峰或同位素离子峰丰度比等方式,对可能呈现的[M+H]+、[M+Na]+、氯取代或溴取代特征碎片离子进行判别。综上,研究可为蔬菜中11种农药残留的监控和风险评估等提供一种快速、高效和可靠的分析手段。10.0 g eggplant were homogenized with acetonitrile,cleaned up with PSA,GCB,MgSO4 and NaCl,and then a rapid pretreatment method coupled with QuEChERS-HPLC∕MRM-IDA-EPI was established to identify the compounds’structures and reasonable fragmentation ions of 11 pesticide residues in eggplant,and directly injected for analysis using+MRM-IDA-EPI mode with external standardized quantification.The results showed that the method appeared to be a good linear relationship in the concentration ranges of 10—250μg∕L,with correlation coefficients(r)between 0.9949 and 0.9999.The average recoveries(P)at the concentration levels of 0.01—0.25 mg∕kg were determined in the range of 69.02%—127.49%with relative standard deviations(RSD)between 1.48%and 13.56%.Simultaneously,the method could be detected[M+H]+,[M+Na]+,Cl or Br characteristic fragment ions through EPI structure analysis on molecular ion,sodium ion or isotopic ion.In conclusion,this method could provide a fast,efficient and reliable analysis method for the monitoring and risk assessment of 11 pesticide residues in vegetables to avoid false positives in qualitative analysis.

关 键 词：高效液相 多反应监测-信息依赖-增强型质谱 茄子 农药残留 同位素离子峰 

分 类 号：S481.8[农业科学—农药学]