基于UPLC-TQ/MS联用技术分析乳香配伍没药后对乳香中化学成分溶出的影响  

Dissolution of the chemical components in combination of frankincense with myrrha based on UPLC-TQ/MS method

作　　者：项想 潘承蓉 高茹梦 宿树兰[1] 曾慧婷 朱振华[1] 钱大玮[1] 段金廒[1,2] XIANG Xiang;PAN Cheng-rong;GAO Ru-meng;SU Shu-lan;ZENG Hui-ting;ZHU Zhen-hua;QIAN Da-wei;DUAN Jin-ao(Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, National and Local Collaborative Engineering Center of Chinese Medicinal Resources Industrialization and Formulae Innovative Medicine, and Jiangsu Key Laboratory for High Technology Research of TCM Formulae, Nanjing University of Chinese Medicine, Nanjing 210023, China;State Key Laboratory Cultivation Base for TCM Quality and Efficacy, Nanjing University of Chinese Medicine, Nanjing 210023, China)

机构地区：[1]南京中医药大学中药资源产业化与方剂创新药物国家地方联合工程研究中心/江苏省中药资源产业化过程协同创新中心/江苏省方剂高技术研究重点实验室,南京210023 [2]南京中医药大学中药品质与效能国家重点实验室(培育),南京210023

出　　处：《药物分析杂志》2018年第4期590-597,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然科学基金项目(No.30973885);教育部优秀人才计划项目(No.NCET-13-0873);江苏省方剂高技术研究重点实验室开放课题资助项目(No.FJGJS-2015-12)

摘　　要：目的:建立同时测定乳香中11个化学成分的UPLC-TQ/MS方法,并进一步分析乳香、没药配伍后乳香中化学成分的溶出变化,以期从化学成分角度阐明二者配伍的合理性。方法:应用UPLC-TQ/MS联用技术对乳香及药对中的萜类成分进行分析。采用Acquity^(TM) UPLC BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm),以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.4 m L·min^(-1);采用UPLC-TQ-MS的电喷雾正、负离子源(ESI+/ESI-),多反应监测(MRM)模式。结果:乳香配伍没药后乳香中β-乳香酸、3α-乙酰基-甘燧-7,24二烯-21-酸、羽扇20(29)烯-3α-乙酰基-24-酸、3-乙酰基-11-酮基-β-乳香酸含量分别由0.919%、1.103%、0.178%、1.365%上升至1.156%、1.916%、0.220%、1.752%;α-乳香酸、3β-乙酰氧基-5α-8,24-羊毛脂二烯-21-酸、乙酰11α-甲氧基-β-乳香酸、3α-乙酰氧基-羊毛脂-8,24-二烯-21-酸、3-羟基甘燧烷-8,24-二烯-21-酸含量分别由0.553%、0.334%、1.010%、0.815%、1.071%下降至0.505%、0.210%、0.534%、0.622%、0.971%。结论:乳香配伍没药后,乳香中的化学成分溶出发生变化,该研究结果为进一步阐明二者配伍协同增效的物质基础提供了科学依据。Objective：To establish a method for simultaneous determination of eleven components in frankincense by UPLC-TQ/MS and to explore the dissolution variation of the components after combination with myrrha.To explain the material basis of the herbal pair.Methods：The UPLC-TQ/MS determination of terpenoids in frankincense and the herbal pair was performed on an Acquity^TM UPLC BEH C18（2.1 mm×50 mm,1.7 μm） column with the mobile phase consisting of 0.1% formic acid-acetonitrile（gradient elution）.Both the positive and negative scanning modes were applied in the follow-up analysis.Then,multiple reaction monitoring（MRM） was applied.Results：After compatibility,the contents of β-boswellic acid,3α-acetoxy-tirucall-7,24-dien-21-oic acid,3α-acetyl-20（29）-lupene-24-oic acid and 3-acetyl-11-keto-β-boswellic acid in frankincense were increased from 0.919%,1.103%,0.178% and 1.365% to 1.156%,1.916%,0.220% and 1.752%.The contents of α-boswellic acid,3β-acetoxy-5α-lanosta-8,24-dien-21-oic acid,acetyl 11α-methoxy-β-boswellic acid,3α-acetyloxylanosta-8,24-dien-21-oic acid and 3-keto-tirucall-8,24-dien-21-oic acid were decreased from 0.553%,0.334%,1.010%,0.815% and 1.071% to 0.505%,0.210%,0.534%,0.622% and 0.971%.Conclusion：Being compatible with myrrha,the dissolution of the chemical constituents in frankincense has changed.This study may provide a scientific foundation for explaining the material basis of the herbal pair of frankincense and myrrha.

关 键 词：乳香-没药 树脂 中药配伍 化学成分溶出 超高效液相色谱仪串联三重四极杆质谱 

分 类 号：R917[医药卫生—药物分析学]