基于UPLC-TQ/MS联用技术分析乳香-没药不同比例配伍化学成分溶出变化  

Dissolution changes of chemical components in different compatibility ratio of frankincense and myrrha based on UPLC-TQ/MS method

作　　者：缪晓冬 高茹梦 宿树兰[1] 尚尔鑫[1] 钱大玮[1] 段金廒[1] MIAO Xiao-dong;GAO Ru-meng;SU Shu-lan;SHANG Er-xin;QIAN Da-wei;DUAN Jin-ao(Jiangsu Key Laboratory for High Technology Research of TCM Formulae/Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization/National and Local Collaborative Engineering Center of Chinese Medicinal Resources Industrialization and Formulae Innovative Medicine,Nanjing University of Chinese Medicine,Nanjing 210023,China)

机构地区：[1]南京中医药大学江苏省方剂高技术研究重点实验室江苏省中药资源产业化过程协同创新中心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

出　　处：《药物分析杂志》2019年第10期1800-1810,共11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、没药中16个化学成分的UPLC-TQ/MS方法,对乳香-没药7个不同配伍比例的化学成分溶出变化进行定量分析;从化学成分角度分析乳香、没药不同配伍比例中的化学成分溶出变化,以期确定最优配伍比例,为进一步阐明量效关系和指导临床用药提供依据。方法:应用UPLC-TQ/MS联用技术对乳香-没药不同配伍比例(1∶1,2∶1,1∶2,2∶3,3∶2,3∶4,5∶3)的化学成分溶出变化进行分析。采用AcquityTMUPLC BEH C18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0.3 mL·min^-1,采用UPLC-TQ/MS的电喷雾正、负离子源(ESI^+/ESI^-),多反应检测(MRM)模式。结果:乳香-没药为2∶1配伍的16个化学成分总含量最高(1.664%)且浸膏得率较高(59.56%);16个化合物中,3α-乙酰基-甘燧-7,24-二烯-21-酸(0.146%)、乙酰11α-甲氧基-β-乳香酸(0.079%)、β-乳香酸(0.210%)、3β-乙酰氧基-5α-8,24-羊毛脂二烯-21-酸(0.058%)、3α-乙酰氧基-羊毛脂-8,24-二烯-21-酸(0.197%)在乳香-没药比例为1∶1配伍时含量最高;3-羟基甘遂烷-8,24-二烯-21-酸(0.164%)、3-乙酰基氧基甘遂-8,24-二烯-21-羧酸(0.065%)、松香酸(0.017%)、3-α羟基甘燧烷-7,24-二烯-21-酸(0.140%)在乳香-没药比例为2∶1配伍时含量最高;3-O-乙酰基-α乳香酸(0.189%)在乳香-没药比例为3∶2配伍时含量最高;2-甲氧基-8,12-环氧吉马烷-1(10),7,11-三烯-6-酮(0.265%)、3-乙酰基-11-酮基-β-乳香酸(0.267%)、2-甲氧基-5-乙酰基-呋喃吉马烷-1(10)-烯-6-酮(0.058%)在乳香-没药比例为3∶4配伍时含量最高;α-乳香酸(0.149%)、11-酮基乳香酸(0.036%)在乳香-没药比例为5∶3配伍时含量最高。其中,乙酰11α-甲氧基-β-乳香酸仅在配伍比例为1∶1配伍时检测到,16个化合物在乳香-没药1∶1配伍时全部检测出。结论:乳香-没药不同配伍比例的化学成分溶出不同,且配伍比例为1∶1和2∶1时溶出化学成分种类Objective:To establish an UPLC-TQ-MS method for simultaneous determination of 16 components in frankincense-myrrha compatibility for quantitative analysis of dissolution changes of chemical components in 7 different compatibility ratios of frankincense and myrrha,with an expectation to determine the optimal compatibility ratio for further clarification of the dose-effect relationship and guidance for clinical medication. Methods:Dissolution changes of chemical components in different compatibility ratios of frankincense and myrrha(1∶1,2∶1,1∶2,2∶3,3∶2,3∶4 and 5∶3) were determined by UPLC-TQ/MS. The separation was performed on an AcquityTM UPLC BEH C18(2.1 mm×50 mm,1.7 μm) column. And the mobile phase consisted of 0.1% formic acid-acetonitrile with gradient elution at a flow rate of 0.3 mL·min^-1. Both the positive and negative scanning modes were applied in the multiple reaction monitoring(MRM). Results:The total contents of 16 chemical components(1.664%) and the extract yield(59.56%) were highest in frankincense-myrrha with 2∶1 compatibility. Among 16 compounds,3α-acetoxy-tirucall-7,24-dien-21-oic acid(0.146%),acetyl 11α methoxy-β-boswellic acid(0.079%),β-boswellic acid(0.210%),3β-acetoxy-5α-lanosta-8,24-dien-21-oic acid(0.058%) and 3α-acetyloxy-lanosta-8,24-dien-21-oic acid(0.197%) were most abundant in frankincense-myrrha with 1∶1 compatibility. 3-hydroxytirucall-8,24-dien-21-oic acid(0.164%),3-acetyloxytirucall-8,24-dien-21-oic acid(0.065%),abietic acid(0.017%)and 3α-hydroxy tirucall-7,24-dien-21-oic acid(0.140%) were most abundant in frankincense-myrrha with 2∶1 compatibility. 3-O-acetyl-α-boswellic acid(0.189%) was most abundant in frankincense-myrrha with 3∶2 compatibility. 2-methoxy-8,12-epoxygermacra-1(10),7,11-trien-6-one(0.265%),3-acetyl-11-keto-β-boswellic acid(0.267%) and 2-methoxy-5-acetoxyfruranogermacr-1(10)-en-6-one(0.058%) were most abundant in frankincense-myrrha with 3∶4 compatibility. α-boswellic acid(0.149%) and 11-keto-boswellic acid(0.036%) were most ab

关 键 词：乳香-没药 树脂 配伍比例 化学成分溶出 物质基础 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]