UPLC-MS/MS法同时测定保健品中11种非法添加药物  

Simultaneous determination of 11 illegally added drugs in healthcare foods by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：王颖[1] 贾丽[1] 朱琳娜[1] 冯月超[1] 马立利[1] 王建凤[1] 范筱京[1] WANG Ying, JIA Li, ZHU Lin-na, FENG Yue-chao, MA Li-li, WANG Jian-feng, FAN Xiao-jing(Beijing Center for Physical and Chemical Analysis, Beijing Engineering Research Center of Food Safety Analysis, Beijing 10008)

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：《食品科技》2018年第5期327-331,共5页Food Science and Technology

基　　金：北京市科学技术研究院萌芽计划项目(2015-03)

摘　　要：建立了一种同时检测改善睡眠类、辅助降压类和减肥类保健品中11种非法添加药物的超高效液相色谱-串联质谱分析方法。样品经50%甲醇-水溶液提取,BEH C18色谱柱分离,用0.1%甲酸乙腈溶液和0.1%甲酸水溶液进行梯度洗脱,质谱采用多反应监测模式对11种非法添加药物的定量离子和定性离子进行监测。在10 min内完成了阿替洛尔、卡托普利、佐匹克隆、哌唑嗪、褪黑素、文拉法辛、氯美扎酮、酚酞、阿普唑仑、N-单去甲基西布曲明和利血平11种非法添加药物的分离分析。11种非法添加药物在3个添加水平的回收率为78.3%~105%,相对标准偏差小于9.6%(n=6),方法定量限均小于15μg/kg。该方法简便、快速、灵敏度高,适合改善睡眠类、辅助降压类和减肥类保健品中11种非法添加药物的测定。UPLC-MS/MS was proposed for simultaneous determination of 11 illegally added drugs, including sleep-improving, hypotensives and antiobesics, in health-care food. Samples were extracted with 50% methanol aqueous solution. The separation was performed on a Waters ACQUITY UPLC BEH C18 column（50 mm×2.1 mm,1.7 μm） by using 0.1%（v/v） formic acid acetonitrile and 0.1%（v/v） formic acid solution as the mobile phases with gradient elution.Using LC-MS/MS with multiple reactions monitoring（MRM）, identification of the major components of the 11 kinds of illegally added drugs were performed based upon the intensities of fragments. The recoveries were ranged from 78.3% to 105% for the 11 kinds of illegally added drugs with 3 spiked. The relative standard deviations（RSDs） were less than 9.6%（n=6）, and the limits of quantitation（LOQ） for the 11 kinds of illegally added drugs were less than 15 μg/kg. The proposed method is fast, accurate and sensitive, which is suitable for detecting 11 kinds of illegally added drugs in in health-care foods.

关 键 词：非法添加药物 超高效液相色谱-串联质谱 保健品 

分 类 号：O657.63[理学—分析化学]