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自组装管尖固相萃取/超高效液相色谱-高分辨质谱法测定水果中的15种酸性农药

邱楠楠 董桂贤 陈达炜 周爽 赵云峰

分析测试学报2017,Vol.36Issue(1):31-36,6.
分析测试学报2017,Vol.36Issue(1):31-36,6.DOI:10.3969/j.issn.1004-4957.2017.01.005

自组装管尖固相萃取/超高效液相色谱-高分辨质谱法测定水果中的15种酸性农药

Determination of 15 Acidic Pesticides in Fruit by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry with a Self-assembly Pipette Tip Solid-phase Extraction

邱楠楠 1董桂贤 2陈达炜 1周爽 1赵云峰1

作者信息

  • 1. 国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室,北京100021
  • 2. 烟台市疾病预防控制中心,山东烟台264003
  • 折叠

摘要

Abstract

A self-assembly pipette tip solid-phase extraction (PTSPE)/high-resolution benchtop Q Exactive mass spectrometric(HRMS) method for the analysis of 15 acidic pesticides in fruit was established.The samples were first extracted with 1% formic acid in acetonitrile,and then the extracts were cleaned up using PTSPE procedure with the adsorbent of PEP and HILIC.The chromatographic analysis was performed on a T3 column.And the qualitative and quantitative analyses were performed under tSIM/ddMS2 mode by high resolution mass spectrometry.The internal standard calibration was used for quantification,and the method showed a good linearity (r2 > 0.99) in a certain concentration range for the 15 acidic pesticides.The limits of quantitation(LOQ) were between 0.2 μg/kg and 10 μg/kg.The recoveries of the analytes in apples,cherry tomatoes and strawberries samples at spiked levels of LOQ,10 μg/kg and 100 μg/kg ranged from 73.5% to 115.9%,with relative standard deviations(RSDs) of 1.0%-8.3%.The results showed that the method was sensitive and accurate,and was suitable for the analysis of acidic pesticides in fruit.

关键词

管尖固相萃取/超高效液相色谱-高分辨质谱法/水果/酸性农药

Key words

pipette tip solid-phase extraction(PTSPE)/ultra high performance liquid chromatography-high resolution mass spectrometry(UPLC-HRMS)/fruit/acidic pesticides

分类

化学化工

引用本文复制引用

邱楠楠,董桂贤,陈达炜,周爽,赵云峰..自组装管尖固相萃取/超高效液相色谱-高分辨质谱法测定水果中的15种酸性农药[J].分析测试学报,2017,36(1):31-36,6.

基金项目

国家食品安全风险评估中心高层次人才队伍建设523项目 ()

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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