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

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

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

High performance liquid(HPLC)Multi reaction monitoring-information dependent acquisition-Enhanced Product Ion(MRM-IDA-EPI)EggplantPesticide residueIsotopic ion

汤逸飞、屠雨晨、陈欣慰、黄芳、张国平

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嘉兴市农业综合检验检测中心,嘉兴 314050

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

全国农产品质量安全检验检测体系建设项目嘉兴市公益性研究计划项目桐乡市重点科技计划项目

浙农计发20157号2021AY10082202201062

2024

上海农业学报
上海市农业科学院,上海市农学会

上海农业学报

CSTPCD
影响因子:0.434
ISSN:1000-3924
年,卷(期):2024.40(3)
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