UPLC-ESI-HRMS同时测定藏药小大黄及其炮制品中11种成分  

Simultaneous determination of 11 components in raw and processsed products of Rheum pumilum roots by UPLC-ESI-HRMS

作　　者：高元平 加多五尼 吕金盈 高宇明 董红娇 李源 吴秀清 曾锐 GAO Yuan-ping;JIA Duo-wu-ni;LV Jin-ying;GAO Yu-ming;DONG Hong-jiao;LI Yuan;WU Xiu-qing;ZENG Rui(School of Pharmacy,Southwest Minzu University,Chengdu 610041,China;Ziyang Institute for Food and Drug Control,Ziyang 641300,China)

机构地区：[1]西南民族大学药学院,四川成都610041 [2]资阳市食品药品检验所,四川资阳641300

出　　处：《中草药》2020年第22期5730-5736,共7页Chinese Traditional and Herbal Drugs

基　　金：国家重点研发计划项目(2017YFC1700705);四川省留学人员科技活动项目择优资助经费计划项目(2018-68);四川省重点研发计划项目(2019YFS0174);西南民族大学研究生创新型科研项目(CX2019SZ169)。

摘　　要：目的建立UPLC-ESI-HRMS方法同时测定藏药小大黄Rheumpumilum及酒炙、炒炭、蒸炙3种炮制小大黄中11种成分。方法色谱采用KinetexTM C18色谱柱(150 mm×4.6 mm,2.6μm),流动相为乙腈-0.1%甲酸水溶液,梯度洗脱,体积流量0.3 mL/min,进样量1μL,柱温32℃。质谱采用ESI离子源,负离子模式进行检测。结果所测11种成分没食子酸、表儿茶素、虎杖苷、土大黄苷、木犀草素、大黄素-8-O-β-D-葡萄糖苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚在测定质量浓度范围内具有良好的线性关系,r值均≥0.9991,方法精密度、重复性和稳定性良好,加样回收率在91.31%~107.08%,RSD在1.73%~3.58%。小大黄炮制后没食子酸、虎杖苷、大黄素-8-O-β-D-葡萄糖苷、大黄素含量发生显著变化。在酒炙、炒炭中没食子酸、大黄素含量均显著升高,炒炭中大黄素-8-O-β-D-葡萄糖苷含量显著降低,虎杖苷含量在所有炮制品中均显著降低。结论该方法简单、快速、准确度及灵敏度高,可用于小大黄及其3种炮制品11种成分的测定,为进一步研究小大黄炮制前后化学成分变化奠定基础。Objective To establish an ultra-high performance liquid chromatography coupled with hybrid quadrupole-orbitrap mass spectrometry(UPLC-ESI-HRMS)determination method for simultaneous determination of 11 components from raw,wine-broiled,carbon-fried and steamed Rheum pumilum roots.Methods The chromatographic separation was performed on a KinetexTM C18 column(150 mm×4.6 mm,2.6μm)with a gradient elution of acetonitrile and 0.1%formic acid in water at flow rate 0.3 mL/min,the injection volume was 1μL and column temperature was 32℃.The mass spectrometry was detected using ESI ion source and negative ion mode.Results Eleven components gallic acid,epicatechin,polydatin,rhaponticin,luteolin,emodin-8-O-β-D-glucoside,aloe-emodin,rhein,emodin,chrysophanol and physcion showed a good linear relationship within a certain concentration range.The precision,repeatability and stability of the method were good for the determination of 11 components.The average recoveries varied between 91.31%and 107.08%and the RSD were between 1.73%and 3.58%.The content of gallic acid,polydatin,emodin-8-O-β-D-glucoside and emodin changed in processsed products of R.pumilum roots.The content of gallic acid and emodin increased significantly in the wine-broiled and carbon-fried process.The content of emodin-8-O-β-D-glucoside in the carbon-fried process was significantly reduced,and the content of polydatin was significantly reduced in all processed products.Conclusion This determination method is simple,stable,accurate and reliable.It can be applied for rapid quantitative determination of 11 components in raw and processsed products of R.pumilum,which laid the foundation for further research on R.pumilum roots.

关 键 词：小大黄 炮制品 酒炙 炒炭 蒸炙 UPLC-ESI-HRMS 没食子酸 表儿茶素 虎杖苷 土大黄苷 木犀草素 大黄素-8-O-β-D-葡萄糖苷 芦荟大黄素 大黄酸 大黄素 大黄酚 大黄素甲醚 

分 类 号：R283.6[医药卫生—中药学]