高效液相色谱串联静电轨道离子阱质谱筛查奶粉中16种磺胺类药物  

Screening of 16 sulfonamides in infant formula with ultra performance liquid chromatography combined with high resolution mass spectrometry

作　　者：王震 陈琦[3] 李远颂 李奇峰 储晓刚[1,4] WANG Zhen;CHEN Qi;LI Yuan-song;LI Qi-feng;CHU Xiao-gang(College of Precision Instrument and Opto-Electronics Engineering , Tianjin University, Tianjin 300071;Chinese Academy of Inspection and Quarantine, Beijing 100176;Huangshan Customs of People's Republic of China, Huangshan 230022;Ausnutria Dairy ( China) Corporation Ltd.,Changsha 410005)

机构地区：[1]天津大学精密仪器与光电子工程学院,天津300071 [2]中国检验检疫科学研究院,北京100176 [3]中华人民共和国黄山海关,黄山230022 [4]澳优乳业(中国)有限公司,长沙410005

出　　处：《分析试验室》2019年第6期675-679,共5页Chinese Journal of Analysis Laboratory

基　　金：北京市自然科学基金北京三元食品股份有限公司联合资助项目(S150008);国家自然科学基金项目(21305101,61378048)资助

摘　　要：建立了超高效液相色谱串联高分辨质谱Q-Exactive快速定性筛查婴幼儿奶粉中16种磺胺类药物残留的方法。2 g奶粉样品以6 mL乙腈和4 mL水为溶剂提取,均质震荡后,使用无水硫酸镁脱水,离心后取乙腈层用100 mg C18固相吸附剂净化,并采用针头式滤膜过滤进样。本方法以FullMS/AIF (数据非依赖模式)扫描样品信息,FullMS/ddms^2(数据依赖)模式建立包含保留时间、母离子质核比、碎片离子信息的磺胺药物的数据库,利用Tracefinder软件对样品中残留的磺胺类药物进行快速的定性和定量。结果表明,16种磺胺类药物在10,50,100μg/kg添加水平内,平均加标回收率为67%~116%,RSD为1. 8%~12%,在各自的考察浓度范围内线性关系良好,R> 0. 99。Screening method of 16 sulfonamides residues in infant formula was established by using high performance liquid chromatography coupled with high resolution mass spectrometry Q-exactive. Infant formula (2g) was extracted with 6 mL acetonitrile and 4 mL water. After homogenous shock, the solution was dehydrated with anhydrous magnesium sulfate, and the layer of acetonitrile was purified with 100 mg C18 after centrifugation. Samples were filtered by needle filter membrane before analysis. Screening information database was established by scanning model of FullMS/AIF and FullMS/ddms^2, which contained retention time, mother ion mass ratio, sulfonamide fragment ions. Thus, using Trace Finder software, qualitative and quantitative analysis for sulfonamides residues in samples were achieved efficiently. The results showed that the spiked recoveries were 67%- 116%, with RSDs of 1. 8%-12% at the level of 10,50 and 100 μg/kg for 16 sulfonamides.

关 键 词：高分辨质谱Q-Exactive 筛查 磺胺类药物 婴幼儿奶粉 

分 类 号：O657.63[理学—分析化学]