Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2013, Vol. 31 ›› Issue (8): 739-746.DOI: 10.3724/SP.J.1123.2013.01036

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Determination of 30 organochlorine pesticides in animal-originated food products using combined purification by gel permeation chromatography and solid-phase extraction coupled with gas chromatography-mass spectrometry

DU Juan1,2, LÜ Bing2, ZHU Pan2,3, MIAO Hong2, WU Yongning1,2   

  1. 1. College of Food Science and Engineering, Wuhan Polytechnic University, Wuhan 430023, China;
    2. Key Laboratory of Food Safety Risk Assessment, Ministry of Health; China Center for Food Safety Risk Assessment, Beijing 100021, China;
    3. Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330031, China
  • Received:2013-01-18 Revised:2013-03-14 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

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Abstract:

A new analytical method was developed for the determination of 30 organochlorine pesticides (OCPs) in animal-originated food, including pork, chicken, fish and shrimp. The combined purification by gel permeation chromatography (GPC) and solid-phase extraction (SPE) were established by optimizing different fraction collection times. The detection conditions can be achieved by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM). Isotopic internal standards were used for the quantitative determination of the 30 OCPs. The sample pretreatment procedure was based on acetonitrile extraction and combined purification of GPC and Florisil SPE cartridge. The experimental results showed that the linear ranges for 30 OCPs were 5.0-500.0 μg/L, the correlation coefficients were better than 0.996, and the method detection limits (MDLs) of the 30 OCPs were 0.2-2.7 μg/kg. The spiked recoveries at three levels of 5.0, 10.0 and 20.0 μg/kg using pork, chicken, fish and shrimp samples as blank matrices were in the range of 55.0%-119.1%, the relative standard deviations (RSDs) were in the range of 0.4%-15.0%. The method has the advantages of wide linear range, high sensitivity and efficient clean-up procedure, and consistent with the demand of pesticide routine analysis.

Key words: animal-originated food, gas chromatography-mass spectrometry (GC-MS), multi-residue, organochlorine pesticides

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