Chinese Journal of Chromatography

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Determination of clopidol residues in chicken muscle by gas chromatography-mass spectrometry

LIU Xiangguo1, SU Yijuan2, FANG Binghu1, DING Huanzhong1, HE Limin1*, ZENG Zhenling1, CHEN Zhangliu1   

  1. 1.Department of Pharmacology and Toxicology, College of Veterinary Medicine, South China Agricultural University, Guangzhou 510642, China; 2.Department of Ecology, College of Agriculture, South China Agricultural University, Guangzhou 510642, China
  • Received:2008-07-06 Revised:2008-09-15 Online:2009-01-30 Published:1983-03-25
  • Contact: HE Limin

Abstract: A confirmative method to determine clopidol residues in chicken muscle by gas chromatography-mass spectrometry (GC-MS) was developed. The analyte was extracted with acetonitrile, and then purified with an Alumina-B cartridge column. The drug was derived at 80 ℃ for 60 min with Sylon BFT, and more toluene was added and then applied to GC-MS. The mass spectral characteristics of trimethylsilyl derivative of clopidol were interpreted, and selected ion monitoring (SIM) mode was performed at m/z 212, 214, 248 and 263. The clopidol was qualitatively identified by the ratio of relative abundance of the selected ions and determined quantitatively by SIM mode at m/z 248. In the meantime, the matrix effect was evaluated. The range of linearity was 5.0-500 μg/L with the correlation coefficients better than 0.998, and the detection limit was 0.5 μg/kg (S/N=3) for clopidol. The average recoveries from chicken muscle fortified at 5, 10 and 20 μg/kg were 77.0%, 84.5% and 89.4%, respectively, and the relative standard deviations (RSD) were less than 6.9%. The established method is simple, sensitive and reproducible for the identification and quantification of clopidol residues in chicken muscle tissue.

Key words: chicken muscle , clopidol, residue, gas chromatography-mass spectrometry (GC-MS)