Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (11): 1063-1069.DOI: 10.3724/SP.J.1123.2016.07024

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Determination of nine fluoroquinolone residues in chicken by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

YANG Yanfei1,2, CAO Xumin2,3, LI Xuelian4, SONG Jiande2, SUN Xiaoliang2,3, WANG Shuting2,3, WANG Xiaoyin2,3, LI Lin1, ZHAO Sijun2,3   

  1. 1. College of Animal Science and Technology, Anhui Agriculture University, Hefei 230000, China;
    2. China Animal Health and Epidemiology Center, Qingdao 266032, China;
    3. Livestock and Poultry Products Quality and Safety Risk Assessment Laboratory, Ministry of Agriculture(Qingdao), Qingdao 266032, China;
    4. Qingdao Yebio Biological Engineering Co., Ltd., Qingdao 266032, China
  • Received:2016-07-24 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    National Livestock Quality and Safety Risk Assessment Project (No. GJFP201600706); Innovation Fund of China Animal Health and Epidemiology Center (No. 2014IF-0003FF).

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Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for the determination of nine fluoroquinolone residues in chicken was developed. The samples were extracted with phosphate buffer solution, and cleaned up with MISPE columns. Then the drugs were analyzed on a BEH C18 column by gradient elution with acetonitrile and 0.1% (v/v) formic acid solution as mobile phase. The samples were analyzed in electrospray positive ion mode and multiple reaction monitoring (MRM) mode. The analytes were quantified by external standard method. The specific adsorption of MISPE for the nine fluoroquinolones in chicken samples was investigated. The linear ranges were 0.25-100 μg/L with correlation coefficients (r) greater than 0.9965. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.08 μg/kg and 0.25 μg/kg, respectively. At the spiked levels of 0.25, 2.5, 5.0 μg/kg, the recoveries were 65.8%-112.2% with the intra-RSDs of 0.6%-13.5% and inter-RSDs of 0.5%-14.9%, respectively. The maximum capacities of the MISPE column were 464.7-932.4 μg/L. The method is sensitive, simple and rapid for the simultaneous determination of the nine fluoroquinolone residues.

Key words: chicken, fluoroquinolones, molecularly imprinted solid phase extraction (MISPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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