Chinese Journal of Chromatography ›› 2012, Vol. 30 ›› Issue (02): 141-145.DOI: 10.3724/SP.J.1123.2011.09038

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A novel solid phase extraction column combined with ultra performance liquid chromatography/tandem mass spectrometry for selective enrichment and determination of clenbuterol in pork

MENG Wenying1, GUO Zhimou2, SHEN Weijian3, SHEN Chongyu3, WU Bin3, LIU Yanming4, ZHANG Feifang1*, LIANG Xinmiao1,2   

  1. 1. School of Pharmacy, East China University of Science and Technology, Shanghai 200237, China; 2. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China; 3. Food Laboratory, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 4. Shandong Supervision and Inspection Institute of Product Quality, Jinan 250103, China
  • Received:2011-09-29 Revised:2011-11-08 Online:2012-02-28 Published:2012-03-22

Abstract: A simple and efficient method based on a novel solid phase extraction (SPE) cartridge and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of clenbuterol residue in pork. The minced pork sample was ultrasonically extracted by 5% (v/v) perchloric acid and centrifuged at 10000 r/min for 15 min, then the supernatant was purified by an SMCX cartridge, which is a novel SPE column based on homemade silica matrix with two mixed modes of reversed-phase and strong cation exchange, for the selective enrichment and purification of the analyte. The linear range of the method was 0.25~50 μg/kg with a correlation coefficient of 0.9982. The average recoveries ranged from 62.2% to 72.0% at the three spiked levels of 1.25, 12.5 and 50 μg/kg with the relative standard deviations (RSDs) between 4.2% and 6.1%. The limit of detection (S/N=3) was 0.05 μg/kg. The method is simple, fast and can be extended to enrich and determine β-agonist drugs.

Key words: clenbuterol, pork, SMCX cartridge, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), solid phase extraction (SPE)