Determination of 8 Penicillins Residues in Fishery Products by Dispersive Solid phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)  fishery products  penicillins  dispersive solid-phase extraction
  
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郭萌萌,李兆新,谭志军,吴海燕,韩现芹,冷凯良,翟毓秀 中国水产科学研究院黄海水产研究所
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Abstract:
      A high performance liquid chromatography tandem mass spectrometric(HPLC-MS/MS) method was developed for the simultaneous determination of 8 penicillins(e.g.amoxicillin,ampicillin,penicillin G,penicillin V,oxacillin,cloxacillin,nafcillin and dicloxacillin) residues in fishery products.The penicillin G-D7,as an internal standard,was added into the sample before the extraction.The samples were extracted with acetonitrile-water(80∶20,by volume),and then cleaned up by dispersive solid-phase extraction with C18 dispersant sorbent and filtered through a Mr 10000 cut-off ultrafree microcentrifuge filter.The separation of 8 penicillins were performed on a HyPURITY C18 (2.1 mm×150 mm,3.5 μm) column using a mixture of 0.1% formic acid and acetonitrile containing 0.1% formic acid as mobile phase.The qualitative and quantitative analysis for the analyte were carried out under the selective reaction monitoring(SRM) mode with positive electrospay ionization.Under the optimal conditions,the calibration curves were linear in the range of 1.0-50.0 μg/L for ampicillin,penicillin G and nafcillin,2.5-100.0 μg/L for penicillin V,oxacillin,cloxacillin and dicloxacillin,and 5.0-200.0 μg/L for amoxicillin,respectively,with detection limits of 0.6 μg/kg,1.5 μg/kg and 3.0 μg/kg,respectively.The average spiked recoveries for 8 penicillins were between 74%and 98% with relative standard deviations(RSDs)less than 10%.The proposed method is accurate,sensitive and high-efficient,and is applicable for the determination of penicillins in fishery products.
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