Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (05): 463-467.DOI: 10.3724/SP.J.1123.2012.01020

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Determination of virginiamycin M1 and S1 residues in livestock and poultry products by liquid chromatography-tandem mass spectrometry

QIU Yuanjin*, YANG Fang, LIU Zhengcai, LIN Yonghui, LIU Suzhen   

  1. Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China
  • Received:2012-01-13 Revised:2012-03-13 Online:2012-05-28 Published:2012-06-07
  • Contact: Yuan-Jin QIU

Abstract: A liquid chromatography-tandem mass spectrometry method was established for the determination of virginiamycin M1 and S1 residues in livestock and poultry products. The sample was extracted by methanol-acetonitrile solution (1:1, v/v). The supernatant was diluted with 0.01 mol/L ammonium dihydrogen phosphate solution, then purified and concentrated on an Oasis HLB cartridge. The separation of virginiamycin M1 and S1 was performed on a Luna C18 column with the mobile phases acetonitrile and 5 mmol/L ammonium acetate aqueous solution (containing 0.1% (v/v) formic acid) in a gradient elution mode. The identification and quantification of the drugs were carried out by positive electrospray ionization (ESI+) in the multiple reaction monitoring (MRM) mode using external standard method. The calibration curves showed good linearity in the range of 0.15~10.0 μg/L with correlation coefficients (r2) above 0.999. The limits of quantities (LOQs) were both 0.25 μg/kg. The average recoveries of the two drugs spiked at 0.25, 0.5 and 2.5 μg/kg levels in different matrices were between 71.2% and 98.4%, and the relative standard deviations (RSDs) were between 3.6% and 15.4%. The method is simple, rapid, sensitive and accurate. It is suitable for the confirmation and quantification of virginiamycin M1 and S1 residues in livestock and poultry products.

Key words: livestock and poultry, residue, virginiamycin M1, virginiamycin S1, liquid chromatography-tandem mass spectrometry (LC-MS/MS)