QuEChERS与液相色谱-串联质谱联用检测中药、调味品及外敷药物中去甲乌药碱的含量  

Determination of higenamine in Chinese herbal medicine, condiments, and topical medicine by QuEChERS combined with liquid chromatography-tandem mass spectrometry

作　　者：王晗 汤一铸 赵晓亚 叶诚 郭少飞 罗静 熊露 曹维 吴建安 王鹏 WANG Han;TANG Yizhu;ZHAO Xiaoya;YE Cheng;GUO Shaofei;LUO Jing;XIONG Lu;CAO Wei;WU Jian’an;WANG Peng(Technology Center of Wuhan Customs,Wuhan 430050,Hubei;Hubei Institute of Sport Science,Wuhan 430205,Hubei)

机构地区：[1]武汉海关技术中心,湖北武汉430050 [2]湖北省体育科学研究院,湖北武汉430205

出　　处：《色谱》2019年第10期1036-1041,共6页Chinese Journal of Chromatography

基　　金：国家重点研发计划(2018YFC1603500);湖北省体育局重点领域研究课题(2018A009)~~

摘　　要：针对中药材、调味品及外敷药物中的去甲乌药碱,建立了一种基于QuEChERS前处理与液相色谱-串联质谱(LC-MS/MS)联用的检测新方法。样品经甲酸-乙醇提取、QuEChERS吸附剂净化后,样品溶液引入LC-MS/MS进行分析,在多反应监测模式下检测。该方法的检出限为0.03ng/g,线性范围为0.10~100ng/g,精密度为4.33%(0.50ng/g,n=7)。采用所建立的方法对市售的13种中药、4种调味料及1种藏药贴膏中的去甲乌药碱含量进行了检测,在干荷叶、干莲子、山药、玉竹、淮山、花椒、桂皮及骨痛贴膏中检出去甲乌药碱,其含量分别为9667.6、1183.8、21.5、8.2、8.5、148.6、21.3、173.3μg/kg。对花椒和桂皮进行加标回收试验,回收率在92.6%~109.8%之间,表明所建立的方法具有良好的准确性。综上,该方法具有快速、简便、可靠、可批处理的优点。A method combining QuEChERS with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of higenamine in Chinese herbal medicine, condiments, and topical medicine.The sample was subjected to extraction using a formic acid-ethanol mixture, followed by purification of the QuEChERS sorbents;then, the extraction solution was introduced into the LC-MS/MS system for detection in multiple reaction monitoring (MRM) mode.Under the optimal conditions, the detection limit of the developed method was 0.03 ng/g, and the linear range was 0.10-100 ng/g with a relative standard deviation (RSD) of 4.33%(0.5 ng/g, n =7).The method was then applied to the determination of higenamine in 13 kinds of Chinese herbal medicine, four kinds of condiments, and a topical medicine.Higenamine was detected in dried lotus leaf, dried lotus seed, Chinese yam, Yuzhu, Yam, Sichuan pepper, Cassia, and the topical medicine at 9 667.6 , 1 183.8 , 21.5, 8.2, 8.5, 148.6, 21.3, and 173.3 μ g/kg , respectively.The recoveries of higenamine in Sichuan pepper and cassia was 92.6%-109.8%.In conclusion, the method is fast, simple, reliable, and suitable for use in batch operation.

关 键 词：QUECHERS 液相色谱-串联质谱 去甲乌药碱 中药 调味品 

分 类 号：O658[理学—分析化学]