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UPLC-Q-Orbitrap HRMS法同时测定秦艽炮制前后8种成分

Simultaneous determination of eight components before and after processing of Gentiana crassicaulis by UPLC-Q-Orbitrap HRMS
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摘要 目的建立一种UPLC-Q-Orbitrap HRMS定量分析方法,同时测定秦艽炮制前后8种化学成分(龙胆苦苷、马钱苷酸、獐牙菜苦苷、獐牙菜苷、木犀草素、异牡荆素、芹菜素、山柰酚)含量的变化。方法采用Waters Acquity UPLC BEH C18(100 mm×2.1 mm,1.7 μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,体积流量0.3 mL/min,柱温35℃。质谱采用负离子检测模式进行检测。结果秦艽经清炒、酒炙后环烯醚萜类含量均明显升高,且清炒后龙胆苦苷和马钱苷酸含量具有统计学差异。黄酮类在清炒和酒炙后含量变化不大。2类成分总的含量变化为环烯醚萜类成分含量清炒>酒炙>生品;黄酮类成分含量生品>酒炙>清炒。结论建立的UPLC-Q-Orbitrap HRMS同时测定秦艽炮制前后8种成分的方法准确、稳定,为进一步研究秦艽炮制前后主要成分的变化奠定了基础。 Objective To develop and validate a ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap HRMS) method for simultaneously qualitative and quantitative determination of eight chemical components (gentiopicroside, loganic acid, swertiamarin, sweroside, luteolin, isovitexin, apigenin, and kaempferol) in raw and processed products of Gentiana crassicaulis. Methods Waters Acquity UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm) column was used for gradient elution with methanol-0.1% formic acid in mobile phase. The volume flow was 0.3 mL/min and the column temperature was 35℃. The mass spectrometer was detected using negative ion detection mode. Results After frying and wine frying, the content of iridoid in G. crassicaulis was significantly increased. Statistically, the differences between gentiopicroside and loganic acid after frying were significant. The content of flavonoids changed little after frying and wine frying. The total content changes of the two components were as follows:the content of iridoids:frying > wine frying > raw products;flavonoids content:raw products > wine frying > frying. Conclusion Based on UPLC-Q-Orbitrap HRMS, the quantitative analysis method of eight components of raw and processed products of G. crassicaulis was established, which provided a basis for optimizing the processing technology of G. crassicaulis and improving the clinical curative effect of G. crassicaulis.
作者 李源 高元平 罗昊 李爱暖 吕露阳 徐燕 严亨秀 曾锐 LI Yuan;GAO Yuan-ping;LUO Hao;LI Ai-nuan;LV Lu-yang;XU Yan;YAN Heng-xiu;ZENG Rui(School of Pharmacy,Southwest Minzu University,Chengdu 610041,China;Chengdu Guowei Biological Co.,Ltd.,Chengdu 610041,China)
出处 《中草药》 CAS CSCD 北大核心 2019年第12期2856-2861,共6页 Chinese Traditional and Herbal Drugs
基金 国家重点研发计划(2017YFC1700705) 四川省留学人员科技活动项目择优资助经费计划(2018-68) 四川省科技项目(2018JY0069) 四川省科技项目(2019YFS0174) 西南民族大学中央高校重点项目(2018NZD18) 四川省阿坝州应用技术研究与开发项目(YYJS2017004) 西南民族大学研究生创新型科研项目(CX2019SZ174).
关键词 秦艽 UPLC-Q-Orbitrap HRMS 炮制 龙胆苦苷 马钱苷酸 獐牙菜苦苷 獐牙菜苷 木犀草素 异牡荆素 芹菜素 山柰酚 Gentiana crassicaulis Duthie ex Burk. UPLC-Q-Orbitrap HRMS processing gentiopicroside loganic acid swertiamarin sweroside luteolin isovitexin apigenin kaempferol
作者简介 李源(1994-),硕士研究生,研究方向民族药新制剂、新剂型与新技术研究。Tel:15184341481,E-mail:YuanLi216@I26.com;通信作者:曾锐,副教授,主要从事民族药炮制制剂研究。Tel:(028)8552209,E-mail:rzeng@swun.edu.cn.
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