液质联用法同时测定火锅调料中15种喹诺酮类抗生素  

Simultaneous determination of 15 quinolones in Chinese hotpot ingredient by high performance liquid chromatography-tandem mass spectrometry

作　　者：冯月超[1] 王颖[1] 王建凤[1] 曹沅[1] 贾丽[1] 范筱京[1] 

机构地区：[1]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,北京100089

出　　处：《分析试验室》2016年第8期924-927,共4页Chinese Journal of Analysis Laboratory

基　　金：北京市财政资金项目“创新工程项目Ⅲ-1”(PXM2015_178305_000001)资助

摘　　要：建立了一种测定火锅调料中双氟沙星等15种的喹诺酮类抗生素含量的液质联用方法。样品通过酸性乙腈提取,正己烷除脂净化,旋转蒸发浓缩。采用乙腈和含有0.1%（V：V）甲酸的0.005mol/L乙酸铵溶液为流动相,BEHC18为分离色谱柱,三重四极杆质谱仪检测和多反应监测（MRM）正离子扫描模式（ES＋）。结果15种喹诺酮在5.0-100ng/mL浓度范围内线性良好,相关系数大于0.99,检出限范围0.1-1.5μg/kg,加标回收率范围是72.0%-111.5%,RSD范围2.1%-18%。An ultra-performance liquid chromatography-tandem mass spectrometry（ UPLC-MS） method was developed for the simultaneous determination of 15 qunolones in hotpot ingredient. The samples were extracted with acidic acetonitrile,cleaned-up with hexane,and concentrated with a rotary evaporator. The analytes were separated using acetonitrile and 0. 1% fomic acid- 0. 005 mol / L ammonium acetate as the mobile phase,BEH C18 as the analysis column,and finally detected by tandem mass spectrometry in positive ESI mode. All the linear rangs of 15 qunolones are 5. 0 - 100 ng / m L. The correlation coefficients were above 0. 99,and the average recoveries were 72. 0% - 111. 5%. And the relative standard deviations（ RSD,n = 6） are 2. 1% - 18%. The quantitative limits were 0. 1 - 1. 5 μg / kg. This method was simple,effective and sensitive,which is suitable for the determination and confirmation of 15 qunolones in hotpot ingredient.

关 键 词：液质联用 喹诺酮类 火锅调料 

分 类 号：TS201.6[轻工技术与工程—食品科学]