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Determination of cefonicid in milk by high performance liquid chromatography-tandem mass spectrometry
Pages: 77-80
Year: Issue:  1
Journal: Chemical Research

Keyword:  milkcefonicidhigh performance liquid chromatographymass spectrometry;
Abstract: A method based on high performance liquid chromatography‐tandem mass spectrom‐etry (HPLC‐MS) was established for the determination of cefonicid in milk .The milk sample was extracted with acetonitrile .Then ,samples were centrifuged (10 000 r/min ,10 min) to ob‐tain the supernatant .After that the supernatant was added into acetonitrile‐saturated hexane solutions and shaken to obtain the acetonitrile‐soluble substances which were directly deter‐mined by HPLC‐MS .The separation was performed on an ZORBAX Eclipse XDB‐C18 column (150 mm × 4 .6 mm ,5 μm) with 5 mmol/L ammonium acetate and acetonitrile gradient solu‐tion as the mobile phase at a flow rate of 0 .8 mL/min and 35 ℃ .The sample injection volume was 5 μL .The electrospray source was operated in the negative ion mode ,and monitored in the selective reaction monitoring (SRM ) mode .The concentration of cefonicid in the range of 1 .0 -100 μg/kg was linearly correlated to the peak area ,with correlation coefficients 0 .997 .The lim‐it of detection (LOD ) and limit of quantitation (LOQ) were determined to be 0 .04 μg/L and 0 .15 μg/L ,respectively the recoveries of cefonicid were from 87 .4% to 93 .5% with the relative standard deviations (RSD) of 2 .1% to 4 .5% (n = 6) .
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