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液相色谱-质谱联用法测定牛奶中14种青霉素及相应青霉噻唑酸残留量
引用本文:冯月超,范筱京,贾丽,马立利,张经华. 液相色谱-质谱联用法测定牛奶中14种青霉素及相应青霉噻唑酸残留量[J]. 分析试验室, 2012, 0(9): 67-70
作者姓名:冯月超  范筱京  贾丽  马立利  张经华
作者单位:北京市理化分析测试中心,北京市食品安全分析测试工程技术研究中心
基金项目:北京市科学技术研究院科技萌芽计划培养项目资助
摘    要:利用超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定牛奶中的7种青霉素类抗生素以及7种相应的青霉噻唑酸。样品经乙腈沉淀蛋白,上清液N2吹干后,用水溶解,加入正己烷萃取除去脂肪;提取液经ACQUITY UPLCBEH C18柱分离,乙腈-乙酸铵+甲酸水溶液洗脱。14种物质峰分离良好,定量限范围在5~20μg/kg。在10~50ng/mL质量浓度范围内线性良好,相关系数均大于等于0.999,牛奶中的加标回收率在90%~98%。

关 键 词:青霉素类抗生素  青霉噻唑酸  牛奶  超高效液相色谱-串联质谱

Simultaneous determination of 14 penicillins and penicilloic acids in milk by UPLC-MS/MS
FENG Yue-chao,FAN Xiao-jing,JIA Li,MA Li-li and ZHANG Jing-hua. Simultaneous determination of 14 penicillins and penicilloic acids in milk by UPLC-MS/MS[J]. Chinese Journal of Analysis Laboratory, 2012, 0(9): 67-70
Authors:FENG Yue-chao  FAN Xiao-jing  JIA Li  MA Li-li  ZHANG Jing-hua
Affiliation:(Beijing Centre for Physical and Chemical Analysis,Beijing Engineering Research Center of Food Safety Analysis,Beijing 100089)
Abstract:An ultra performance liquid chromatography tandem mass spectrometric(UPLC-MS/MS) analysis method was established for simultaneous analysis of 7 penicillins and 7 penicilloic acids in milk.The milk sample was precipitated with acetonitrile and the supernatant was dried under nitrogen,the residue was dissolved in water and then extracted with n-hexane.The sample extract was separated on a ACQUITY UPLC BEH C18 column,using a mixture of formic acid in water with ammonium acetate and acetonitrile as the mobile phase.The limits of quantitation were 5-20 μg/kg.The correlation coefficients were above 0.999 within the linear range of 10~50 ng/mL.The average recoveries were 90%~98%.
Keywords:Penicillins  Penicilloic acids  Milk  Ultra performance liquid chromatography-tandem mass
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