UPLC-Q-TOF-MS法鉴定消肿止痛液有效部位的化学成分  

Identification of Chemical Components in Active Fraction of Xiaozhong Zhitong Lotion by UPLC-Q-TOFMS

作　　者：王银洁 刘本臣 刘军 莫家欣 胡安琪 刘嘉琪 冯倩仪 宫凯敏 WANG Yinjie;LIU Benchen;LIU Jun;MO Jiaxin;HU Anqi;LIU Jiaqi;FENG Qianyi;GONG Kaimin(Preparation Center,Yinchuan Hospital of TCM,Yinchuan 750001,China;School of TCM,Guangzhou University of TCM,Guangzhou 510006,China)

机构地区：[1]银川市中医医院制剂中心,银川750001 [2]广州中医药大学中药学院,广州510006

出　　处：《中国药房》2019年第23期3232-3239,共8页China Pharmacy

基　　金：宁夏回族自治区重点研发计划项目（No.2016KJHM112）;宁夏青年科技人才托举工程项目

摘　　要：目的:分析消肿止痛液有效部位的化学成分,为阐明其药效物质基础及将其二次开发为软膏制剂提供依据。方法:采用超高效液相色谱-四级杆-飞行时间质谱联用(UPLC-Q-TOF-MS)法对消肿止痛液有效部位(经D101大孔树脂分离得到的40%乙醇洗脱部位)进行成分分析。色谱条件为采用Hypersil GOLD a Q C18色谱柱,以0.1%甲酸乙腈(A)-0.1%甲酸水(B)为流动相进行梯度洗脱,流速0.4 mL/min,进样量4μL,柱温30℃;质谱条件为采用电喷雾离子源(ESI)在正/负离子扫描模式(ESI+/ESI-)下进行检测,扫描范围100~2000 Da,碰撞能量45/-45 e V,扩展碰撞器能量10/15 e V。获得图谱后收集化合物的精确分子量、保留时间和多级碎片离子信息,通过与对照品质谱信息及参考文献比对进行化学成分鉴定。结果:共鉴定出48个化合物,在ESI+、ESI-检测模式下分别鉴定出9、39个。其中,酚酸类成分10个、苯丙素类成分8个、蒽醌类成分9个、黄酮类成分3个、生物碱类成分7个、鞣质类成分5个、其他类成分6个。结论:UPLC-Q-TOF-MS法可快速、高效、准确地鉴定消肿止痛液有效部位的化学成分,该部位的主要化学成分为酚酸类、苯丙素类、蒽醌类、生物碱类和鞣质类。OBJECTIVE:To analyze chemical components in active fraction of Xiaozhong zhitong lotion,to clarify the material basis of its efficacy,and to provide reference for the second development of ointment preparation.METHODS:UPLC-Q-TOF-MS was adopted to analyze the chemical components of active fraction(40%ethanol elution site separated by D101 macroporous resin)of Xiaozhong zhitong lotion.The determination was performed on Hypersil GOLD a Q C18 column with mobile phase consisted of 0.1%formic acid acetonitrile(A)-0.1%formic acid water(B)(gradient elution)at the flow rate of 0.4 mL/min.The sample size was 4μL,and the column temperature was 30℃.The condition of mass spectrometry was ESI detection in positive and negative scanning ion mode(ESI+/ESI-).The scanning range was 100-2000 Da.The collision energy was 45/-45 eV,and the energy of the extended collider was 10/15 eV.The accurate molecular weight,retention time and multi-stage fragment ion information of the compounds were collected after obtaining the chromatogram,and the chemical components were identified by comparing with the mass spectrum information of reference materials and references.RESULTS:A total of 48 compounds were identified,and 9 and 39 compounds were identified under ESI+/ESI-ion mode,mainly including 10 phenolic acids,8 phenylpropanoids,9 anthraquinones,3 flavones,7 alkaloids,5 tannins and 6 other categories.CONCLUSIONS:UPLC-Q-TOFMS method is rapid,efficient and accurate for identify chemical components from active fraction of Xiaozhong zhitong lotion.Main chemical components of the active fraction are phenolic acids,phenylpropanoids,anthraquinones,alkaloids and tannins.

关 键 词：消肿止痛液 有效部位 超高效液相色谱-四级杆-飞行时间质谱联用法 化学成分 鉴定 

分 类 号：R284.2[医药卫生—中药学]