同位素内标-液相色谱-串联质谱法测定水果中11种农药残留量
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(1.成都市疾病预防控制中心,四川 成都 610041;2.成都中医药大学,四川 成都 611130)

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王炼 男 副主任技师 研究方向为有机污染物残留分析E-mail:septwolvesnjwl@163.com

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中国博士后面上项目(2012M521703)


Determination of 11 agricultural chemical in fruits by liquid chromatography tandem mass spectrometry with isotope internal standard
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(Chengdu Center for Disease Control and Prevention,Sichuan Chengdu 610041,China)

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    摘要:

    建立一种同位素内标-液相色谱-串联质谱测定水果中11种农药的方法。方法 样品用乙腈提取,离心后取上清液旋转蒸发浓缩,经过氨基固相萃取小柱净化后,旋转蒸发至干,流动相溶解样品,用Waters XSelect HSS T3色谱柱(2.1 mm×50 mm,2.5 μm)进行分离,以乙腈和0.2%甲酸溶液作为流动相进行洗脱,内标法测定。结果 本研究建立的方法相对标准偏差(RSD)在4.7%~9.4%之间,样品加标回收率在78.6%~107.4%之间,定量限和检出限分别在0.002~2.2和0.000 4~0.66 μg/kg。结论 本研究建立的分析方法操作简便、结果准确、灵敏度高,可满足实验室对食品中农药残留的检测要求。

    Abstract:

    To establish a method for determination of 11 bactericides and fipronil residues in fruits by liquid chromatography tandem mass spectrometry.Methods The samples were extracted by acetonitrile and then homogenized. The supernatants were separated after centrifuge and nearly dried with rotary evaporation. After the solid phase extraction of amino cartridge, the eluent was dried-up by the rotary evaporation. The analytes were dissolved by the mobile phase and determined by liquid chromatography tandem mass spectrometry. The conditions of separation and mass spectrometry were optioned. Results The relative standard deviations of detection were 4.7%-9.4%, the spiked sample recoveries were 78.6%-107.4%. The limits of quantification and detection were 0.002-2.2 and 0.000 4-0.66 μg/kg.Conclusion The method is simple, accurate, sensitive and could meet the determination requirements of pesticide residues in foods.

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王炼,朱作芳,羊雨婷.同位素内标-液相色谱-串联质谱法测定水果中11种农药残留量[J].中国食品卫生杂志,2016,28(2):209-214.

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  • 收稿日期:2016-01-11
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  • 在线发布日期: 2016-04-20
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