Chinese Journal of Chromatography

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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

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