Simultaneous Determination of 14 Macrolide Drugs Residues in Pork Samples by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction
  
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KeyWord:solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  macrolide drugs  pork
  
AuthorInstitution
WANG Yi-han,WANG Zhan-hua,CHEN Wan-qin,WANG Feng,LIU Zhu Zhejiang Institute for Food and Drug Control
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Abstract:
      An ultra performance liquid chromatography-tandem mass spectrometric method with solid phase extraction was established for the simultaneous determination of 14 macrolide drugs in pork samples.Samples were extracted with 70%(volume fraction) acetonitrile,purified by solid phase extraction using a hydrophilic lipophilic balanced(HLB) polymer,and separated on a C18 column(100 mm×2.1 mm,1.7 μm) with acetonitrile and 01% formic acid-2 mmol/L ammonium acetate solution as mobile phases by gradient elution.The analytes were detected by mass spectrometry in positive ion mode under multiple reaction monitoring(MRM) scanning mode,and quantified by external standard method.Results showed that good linearities for 14 macrolide drugs were obtained in the corresponding mass concentration ranges with correlation coefficients(r2) larger than 0.995.The detection limits and quantitation limits of the method were in the ranges of 0.1-0.8 μg/kg and 0.5-3.0 μg/kg,respectively.Recoveries at low,medium and high spiked levels were in the range of 71.1%-102%,with relative standard deviations(RSD) less than 6.0%.This method could be applied in the analysis of macrolide drugs in pork samples with good accuracy and reliability.
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