高效液相色谱-串联质谱法同时检测镇静安神保健食品中的违法添加药物  

Simultaneous Determination of sedative-hypnotic drugs illegal added in health foods by high performance liquid chromatography coupled with triple quadrupole mass spectrometry

作　　者：陈月龙 Chen Yue-long(Xiamen Hongyi Testing Co.,Ltd,Xiamen,Fujian 361000,China)

机构地区：[1]厦门泓益检测有限公司,福建厦门361000

出　　处：《福建分析测试》2020年第3期45-51,共7页Fujian Analysis & Testing

摘　　要：建立了测定镇静安神保健品中苯二氮卓类、巴比妥类和非典型苯二氮卓类等17种目标物的高效液相色谱-串联质谱分析方法。液体、固体(胶囊和片剂)镇静安神保健食品经有机溶剂萃取后,以Phenomenex Kinetex C18柱(2.1 mm×100 mm,2.6μm)分离,采用HPLC-MS/MS电喷雾电离,多反应监测模式(MRM)检测,以保留时间和子离子丰度比定性,基质匹配外标法定量。结果显示目标物在一定浓度范围内呈现良好的线性关系,检测限为0.0002~0.380μg/kg,定量限为0.001~1.266μg/kg;液体、固体镇静安神食品在两个添加水平的回收率为71.8%~110.1%,相对标准偏差在0.2%~9.2%。本方法灵敏、准确、快速,可用于不同镇静安神保健食品中违法添加药物的检测。A high-performance liquid chromatography-mass spectrometric method was established for the simultaneous de⁃termination of sedative-hypnotic drugs(including benzodiazepines,barbiturates,and atypical benzodiazepines),which were illegal mixed into health foods.Liquid and solid(capsule and tablet)were extracted with methanol,separated on a Phenomenex Kinetex C18 chromatographic column(2.1 mm×100 mm,2.6μm).The detection of analytes was performed by electrospray ionization mass spectrometry under multiple reaction monitoring(MRM)mode.The method was qualitative by retention time and product ion abundance,and quantitative by matrix-match external standard.Results showed that there were good linear relationships for target compounds in the certain concentration range.The limits of detection and lim⁃its of quantitation were in the ranges of 0.0002~0.380μg/kg and 0.001~1.266μg/kg,respectively.The recoveries for analyt⁃ics at two spiked levels were in the range of 71.8%~110.1%with relative standard deviations(RSD)of 0.2%~9.2%.The method was sensitive,accuracy,and rapid,which can be used for detection of sedative-hypnotic drugs illegal added in health foods.

关 键 词：镇静安神保健食品 违法添加药物 高效液相色谱-串联质谱 

分 类 号：O657.72[理学—分析化学]