Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (03): 267-272.DOI: 10.3724/SP.J.1123.2011.11008

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Rapid determination of 40 pesticide residues in fruits using gas chromatography-mass spectrometry coupled with analyte protectants to compensate for matrix effects

XU Xiuli1, ZHAO Haixiang1,2, LI Li1, LIU Hanxia1, REN Heling1, ZHONG Weike1*   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 2. College of Science of Hebei North University, Zhangjiakou 075000, China
  • Received:2011-11-06 Revised:2011-12-29 Online:2012-03-28 Published:2012-05-02

Abstract: A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 40 pesticides in fruits. The effects of adding analyte protectants were evaluated for compensating matrix effects and the impacts on the quantitative results. A new combination of analyte protectants-Polyethylene Glycol 400 (PEG 400) and olive oil combination, which can be dissolved in acetone, was used for the quantitative analysis. The pesticides were extracted from fruit samples with acetonitrile and the extracts were cleaned up using micro-solid phase extraction. A GC-MS method in selective ion monitoring (SIM) mode coupled with large volume injection was finally developed. Using the newly developed analyte protectant combination of PEG 400 and olive oil, a good linearity was obtained in the range of 1~200 μg/L with coefficients better than 0.99, and the detection limits were between 0.1~3.0 μg/L. The mean recoveries of the pesticides were 75%~119% with the relative standard deviation values less than 16.6% except for dimethoate. The performance of the analyte protectants was compared with matrix-matched standards calibration curves in terms of quantitative accuracy. The results showed that the method of adding analyte protectants can replace the matrix-matched standard calibration, and can also reduce the sample pretreatment. When the developed method was used for the analysis of apple, peache, orange, banana, grape and other fruit samples, a good matrix compensation effect was achieved, and thus effectively reduced the bad effects of the water-soluble agents to the gas chromatographic column.

Key words: analyte protectants, fruits, matrix effects, multi-residues, pesticides, gas chromatography-mass spectrometry (GC-MS)