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食品研究与开发:2017,38(13):182-185
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UPLC-MS/MS检测乳品饮料中的四环素类残留
李婷婷1,韦曙光2,彭艳1
(1. 贵州民族大学 化学与生态环境工程学院(民族医药学院),贵州 贵阳 550025;2. 贵州省水利水电勘测 设计研究院,贵州 贵阳 550001)
Analysis Tetracycline Antibiotics Residues in Dairy Beverage by UPLC-MS/MS
LI Ting-ting1, WEI Shu-guang2, PENG Yan1
(1. School of Chemistry and Eco-Environmental Engineering(School of Chinese Pharmacy),Guizhou Minzu University,Guiyang 550025, Guizhou,China; 2. Guizhou Survey & Design Reserch Institute for Water Resources and Hydropower, Guiyang 550001, Guizhou, China)
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投稿时间:2017-02-10    
中文摘要: 建立一种超高效液相色谱-串联质谱法检测乳品饮料中四环素、土霉素、金霉素、强力霉素残留的分析方法。 样品前处理用乙腈沉淀蛋白后,采用 HLB 小柱进行净化和富集。采用 Waters Atalantis T3 色谱柱(2.1 mm×150 mm, 3 μm)分离,以 0.1 %甲酸-乙腈为流动相的梯度洗脱模式下,4 种四环素类抗生素在 1.0 ng/mL~200.0 ng/mL 浓度范围 内线性良好,相关系数 r2 为 0.998 5~0.999 2,检出限为 0.5 μg/kg~2.0 μg/kg,定量限为 1.5 μg/kg~6.0 μg/kg,加标回收率 达到 82.5 %~91.5 %。
Abstract:A ultra high performance liquid chromatography mass spectrometry analysis method was established for the residues determination of tetracycline, oxytetracycline, chlortetracycline and doxycycline in dairy bev- erage. After the sample was treated with acetonitrile, it was concentrated and purified by HLB solid phase ex- traction column. The separation of target compound was performed on a Waters Atalantis T3 chromatographic column(2.1 mm × 150 mm, 3 μm) using 0.1 % formic acid-acetonitrile as mobile phase under gradient elution mode. The linear range of 4 tetracycline antibiotics components was in the range of 1.0 ng/mL-200.0 ng/mL with a correlation coefficient of 0.998 5-0.999 2. The detection limit was 0.5 μg/kg-2.0 μg/kg and the quantitative limit was 1.5 μg/kg-6.0 μg/kg. The recovery rate was 82.5 %-91.5 %.
文章编号:201713039     中图分类号:    文献标志码:A
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