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
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KeyWord:pipette tip solid-phase extraction(PTSPE)  ultra high performance liquid chromatography-high resolution mass spectrometry(UPLC-HRMS)  fruit  acidic pesticides
QIU Nan-nan,DONG Gui-xian,CHEN Da-wei*,ZHOU Shuang,ZHAO Yun-feng 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;2.烟台市疾病预防控制中心
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      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 0.2μg/kg and 10μg/kg.The recoveries of the analytes in apples,cherry tomatoes and strawberries samples at spiked levels of LOQ,10μg/kg and 100μg/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.