超高效液相色谱-串联质谱法同时检测动物组织中15种保水功能药物  

Simultaneous determination of 15 water-holding functional drugs in animal tissues using ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘洪斌[1] 姚喜梅 田亚平[1] 张鹭[1] 蔡英华[1] 姜艳彬[1] 李颖[1] LIU Hongbin;YAO Ximei;TIAN Yaping;ZHANG Lu;CAI Yinghua;JIANG Yanbin;LI Ying(China Animal Disease Control Center,Beijing 102609,China;China Association for Standardization,Beijing 100048,China)

机构地区：[1]中国动物疫病预防控制中心,北京102609 [2]中国标准化协会,北京100048

出　　处：《色谱》2018年第4期400-407,共8页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑重点项目(2014BAD13B05)~~

摘　　要：建立了超高效液相色谱-串联质谱检测动物组织中15种保水功能药物残留的分析方法。样品经含1.0%(v/v)甲酸的乙腈溶液提取和Oasis PRiME HLB SPE柱净化后,采用Acquity UPLC BEH C18色谱柱(50 mm×2.1mm,1.7μm)分离,以甲醇和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,在电喷雾电离(ESI)源、正离子模式下,采用MRM监测模式进行数据采集。在1.0~50.0μg/kg范围内,15种保水功能药物的线性关系良好,相关系数均≥0.994 9;定量限均低于1.0μg/kg。通过添加回收试验表明,动物组织中15种保水功能药物的平均回收率为60.0%~111.0%,批内RSD为0.56%~11.5%,批间RSD为2.31%~14.8%。该方法满足动物组织中该药物多残留的检测要求,为应对动物源性食品中筛查风险隐患和监控非法添加提供了新思路。A method based on ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of 15 water-holding functional drugs in animal tissues.The analytes were extracted with acetonitrile containing 1.0%(v/v)methanol,purified by Oasis PRiME HLB SPE column,and analyzed by Acquity UPLC BEH C18 column(50 mm×2.1 mm,1.7μm)using methanol and 0.1%(v/v)formic acid aqueous solution as the mobile phases.The analytes were detected using an electrospray ionization(ESI)source under the MRM mode.The calibration curves of the analytes were linear in the range of 1.0-50.0μg/kg(r≥0.994 9),and the limits of quantification were all less than 1.0μg/kg in animal tissues.The recoveries of the 15 water-holding functional drugs ranged from 60.0%-111.0%in animal tissue samples,with the intra and inter RSDs of 0.56%-11.5%and 2.31%-14.8%,respectively.The method can meet the requirements for the determination of the drug residues in animal tissues.It provides a new idea to identify potential hazards in animal-derived foods and to monitor illegal addition.

关 键 词：超高效液相色谱.串联质谱 残留 保水功能药物 动物组织 

分 类 号：O658[理学—分析化学]