| 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 |
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| 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(9):67-70. |
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| 作者姓名： | 冯月超 范筱京 贾丽 马立利 张经华 |
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| 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 |
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| 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 |
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| 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%。
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| 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 |
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| 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(9):67-70. |
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| Authors: | FENG Yue-chao FAN Xiao-jing JIA Li MA Li-li and ZHANG Jing-hua |
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| Institution: | (Beijing Centre for Physical and Chemical Analysis,Beijing Engineering Research Center of Food Safety Analysis,Beijing 100089) |
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| 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%. |
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| Keywords: | Penicillins Penicilloic acids Milk Ultra performance liquid chromatography-tandem mass |
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