Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (11): 1172-1177.DOI: 10.3724/SP.J.1123.2012.07044

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Determination of 17 pyrethroid pesticide residues in vegetables by gas chromatography-mass spectrometry with negative chemical ionization

SHEN Weijian1*, CAO Xiaowen2, LIU Yijun1, ZHANG Rui1, FAN Xin1, ZHAO Zengyun1, SHEN Chongyu1, WU Bin1   

  1. 1. Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2. Changzhou Entry-Exit Inspection and Quarantine Bureau, Changzhou 213022, China
  • Received:2012-07-26 Revised:2012-09-19 Online:2012-11-28 Published:2012-11-21

Abstract: A method was established for the determination of 17 pyrethroid pesticide residues in vegetables using QuEChERS (quick, easy, cheap, effective, rugged and safe) clean-up method and gas chromatography-mass spectrometry (GC-MS) with negative chemical ionization (NCI). The pyrethroid pesticides in the sample were extracted with acetonitrile. After QuEChERS clean-up with a mixture of primary secondary amine and graphitized carbon black packings, the extract was analyzed by GC-NCI-MS in selected ion monitoring (SIM) mode. An isotope internal standard of cypermethrin was employed to the quantification. The limits of quantification ranged from 0.02 to 5 μg/kg. The recoveries of the pyrethroid pesticides spiked in three different matrixes (peas, broccoli and Chinese onion green) at four spiked levels of 10, 20, 30 and 100 μg/kg were from 71.0% to 139.0%, and the relative standard deviations were less than 12.8%. This method can be used as a conclusive evidence method of the 17 pyrethroid pesticide residues in vegetables.

Key words: negative chemical ionization mass spectrometry (NCI-MS), pyrethroid pesticides, vegetables, gas chromatography (GC)