FOOD SCIENCE ›› 2009, Vol. 30 ›› Issue (12): 157-161.doi: 10.7506/spkx1002-6630-200912032

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Reversed Phase High Performance Liquid Chromatographic Determination of 7 Tetracyclines Residues in Bovine Milk

SHE Yong-xin1,2，LIU Jiang-ying3，LU Xiao-ling1，WANG Jing1,* CAO Wei-qiang4   

  1. (1. Institute of Quality Standards and Testing Technology for Agri-products, Chinese Academy of Agricultural Science, Beijing
    100081, China；2. Institute of Veterinary and Animal Husbandry, Tibet Academy of Agricultural and Animal Husbandry Sciences,
    Lhasa 850009, China；3. Tibet Central Hosptal for Judicial, Lhasa 850000, China；4. Huizhou Entry-Exit Inspection and
    Quarantine Bureau, Huizhou 450012, China)
  • Received:2008-09-08 Revised:2008-12-12 Online:2009-06-15 Published:2010-12-29
  • Contact: WANG Jing1,* E-mail:w_jing2001@126.com

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Abstract:

Residues of 7 tetracyclines were extracted with 0.1mol/L EDTA-McIlvaine buffer solution (pH 3.8) from bovine milk, pretreated with 50% trichloroacetic acid solution, and then subjected to cleanup with HLB solid phase extraction (SPE) cartridge. The analysis of 7 tetracyclines residues was conducted by reverse phase high-performance liquid chromatograph on a sunfireTM C18 column (250 mm × 4.6 mm, 5 μm i.d) with methanol - acetonitrile - 0.01 mol/L oxalic acid solution as a mobile phase (gradient elution) at the flow rate of 1.0 ml/min. The results showed that the method presented a wide-range high-linearity for analyzing these tetracyclines. The peak area was positively correlated with sample solution concentration in the range of 0.05 － 1.0 μg/ml. The average recovery was 78.66% － 106% and the lowest detection limit was 0.02 μg/ml. The method is sensitive, reliable and easy-operating, and can be used for simultaneous determination of 7 tetracyclines residues in bovine milk within 14 minutes.

Key words: RP-HPLC, tetraeyclines, gradient elution, bovine milk

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