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
汤逸飞 1屠雨晨 1陈欣慰 1黄芳 1张国平1
作者信息
- 1. 嘉兴市农业综合检验检测中心,嘉兴 314050
- 折叠
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10-250 μg/L茄子加标基质内线性关系良好,回归方程相关系数(r)为0.994 9-0.999 9;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.
Abstract
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 10-250 μg/L,with correlation coefficients(r)between 0.994 9 and 0.999 9.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Key words
High performance liquid(HPLC)/Multi reaction monitoring-information dependent acquisition-Enhanced Product Ion(MRM-IDA-EPI)/Eggplant/Pesticide residue/Isotopic ion引用本文复制引用
基金项目
全国农产品质量安全检验检测体系建设项目(浙农计发20157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)
出版年
2024
国家科技期刊平台
NSTL
万方数据