超高效液相色谱-串联质谱法测定动物源性食品中的三甲氧苄氨嘧啶  

Determination of trimethoprim in animal origin food by ultra performance liquid chromatographytandem mass spectrometry

作　　者：高洋洋[1] 张朝晖[1] 卢晓宇[1] 严华[1] 何悦[1] 刘鑫[1] 云环[1] 

机构地区：[1]北京出入境检验检疫局技术中心,北京100026

出　　处：《分析试验室》2014年第3期315-318,共4页Chinese Journal of Analysis Laboratory

基　　金：质检总局科技项目(20BIK146);国家高技术研究发展计划(863计划;2012AA101603)资助

摘　　要：建立了一种超高效液相色谱-串联质谱法（UPLC—MS／MS）测定多种基质（鸡肉、鱼肉、鸡肝、鸡蛋和牛奶）中三甲氧苄氨嘧啶的分析方法。样品用甲酸-乙腈（1：9，V／V）溶液提取，正己烷除脂净化，AcquityUPLCBEHC，8柱（1．7μm，2．1mm×50mm）分离，以甲醇和体积分数0．1％甲酸5mmol乙酸铵（V/V）作为流动相进行梯度洗脱，电喷雾正离子（ESI＋）模式电离，多反应监测（MRM）模式检测。结果表明：三甲氧苄氨嘧啶质量浓度在1．25～15．0μg/L范围内线性关系良好（r≥0．99）。方法的定量限（信噪比为10）为5．0μg／kg，在5．0，10．0μg／kg添加浓度的回收率为61．2％～108．5％，相对标准偏差（n=6）在1．4％～9．8％之间。方法适合于多种基质中三甲氧苄氨嘧啶的测定。A method for the determination of trimethoprim in different animal origin food matrices （including chicken muscle, fish muscle, chicken liver, egg and milk） has been developed by ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）. Samples were extracted by formic acid-acetonitrile （1：9, V/V）, cleaned by hexane, separated on an Aequity UPLC BEH Cls column （2. 1 mm ×50 mm, 1.7 μm） with a gradient elution. The determination was carried by mass spectrometry with electrospray ion source in the positive mode and monitored by the multiple reaction monitoring （MRM） mode. The calibration curve showed a good linearity in the range of 1.25 - 15.0 μg/L, and the correlation coefficient （r） was higher than 0. 99. The limit of quantification （LOQ, S/N = 10） for trimethoprim was 5.0μg/kg. At the spiked levels of 5.0 and 10. 0 μg/kg, the recoveries of trimethoprim ranged from 61.2% to 108.5%, and the relative standard deviation （ RSD, n = 6） analysis of trimethoprim ranged from 1.4% to 9.8%. The mothed is suitable for the qualitative and quantitative in multiple matrices.

关 键 词：超高效液相色谱-串联质谱 三甲氧苄氨嘧啶 动物源性食品 

分 类 号：O657.63[理学—分析化学]