色谱

色谱

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分散固相萃取-超高效液相色谱-串联质谱法测定果蔬、牛奶、植物油和动物肌肉中残留的61种有机磷农药

叶瑞洪1*, 苏建峰2   

  1. 1. 福建师范大学福清分校, 福建 福清 350300; 2. 福建华日食品安全检测有限公司, 福建 福州 350015
  • 收稿日期:2011-04-14 修回日期:2011-05-17 出版日期:2011-07-28 发布日期:2011-08-19
  • 通讯作者: 叶瑞洪,副教授,研究方向为分析化学. Tel: (0591)85254164
  • 基金资助:

    福建省教育厅项目(JB09243)和食品安全分析与检测教育部重点实验室（福州大学）开放课题（FS1108）

Determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

YE Ruihong1*, SU Jianfeng2   

  1. 1. Fuqing Branch of Fujian Normal University, Fuqing 350300, China; 2. Fujian Fairreach Food Safety Testing Co., Ltd., Fuzhou 350015, China
  • Received:2011-04-14 Revised:2011-05-17 Online:2011-07-28 Published:2011-08-19

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摘要： 建立了果蔬、牛奶、植物油和动物肌肉中61种有机磷农药多残留的分析方法。果蔬和牛奶样品用乙腈均质提取,盐析分配;植物油样品用正己烷溶解,乙腈萃取;动物肌肉样品用正己烷配合乙腈-水溶液均质提取,盐析分配。各提取法得到的提取液采用C18和Primary Secondary Amine (PSA)粉末分散固相萃取净化,超高效液相色谱-串联质谱仪(UPLC-MS/MS)分析,采用电喷雾离子化正离子方式(ESI+)及多反应监测模式(MRM)测定,基质匹配标准溶液外标法定量。方法的定量限(S/N≥10)均达到0.01 mg/kg;回收率为62.8%～107%,相对标准偏差为4.2%～19%。该方法准确、灵敏、快速,可满足多种食品中有机磷农药残留的检测要求。

关键词: 残留, 超高效液相色谱-串联质谱法, 动物肌肉, 分散固相萃取, 果蔬, 牛奶, 有机磷农药, 植物油

Abstract: A dispersive solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles. The fruit, vegetable and milk samples were extracted with acetonitrile and separated with salting out method; vegetable oil samples were dissolved by n-hexane, and extracted with acetonitrile; animal muscle samples were extracted with acetonitrile-water assisted by n-hexane and separated with salting out method. And then the supernatants were purified using dispersive solid-phase extraction (C18 and primary secondary amine powder) prior to the UPLC-MS/MS analysis. The analytes were indentified in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Under the optimal conditions, the detection limits (S/N≥10) of the method were 0.01 mg/kg. The recoveries were 62.8%~107%, and the relative standard deviations (RSDs) were in the range of 4.2%~19%. The method has the advantages of easy, fast, and more sensitive, and can meet the requirement of the determination of organophosphorous pesticide residues in the foods.

Key words: animal muscles, fruits, organophosphorous pesticides, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), vegetable oils, vegetables, dispersive solid-phase extraction, milk, residues