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基于UPLC-Q-TOF-MS/MS快速分析亚大黄中的抗补体活性成分 被引量:8

Rapid Analysis of Anti-complement Constituents in Rheum ihasaense Based on UPLC-Q-TOF-MS/MS
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摘要 目的:通过UPLC-Q-TOF-MS/MS技术快速分析亚大黄中的抗补体活性成分群,为阐明亚大黄的抗补体活性药效物质基础提供参考。方法:对亚大黄95%醇提物进行萃取得到石油醚、乙酸乙酯、正丁醇3个部位,并测定3个部位经典途径的抗补体溶血活性(CH50);采用UPLC-Q-TOF-MS/MS对3个部位分别进行化学成分的表征,使用质谱分析软件中的目标化合物筛查法,通过保留时间、精确相对分子质量和二级质谱裂解碎片鉴定化学成分。结果:亚大黄正丁醇部位抗补体活性为0.032 g·L^-1,强于阳性药肝素钠;在优化的LC-MS条件下,结合Scifinder数据库、对照品和相关文献,鉴定了石油醚部位主要成分9个,主要是脂肪酸及甾醇类化合物;鉴定了乙酸乙酯部位主要成分13个,主要是游离蒽醌类和二苯乙烯类;鉴定了正丁醇部位主要成分25个,主要是蒽醌苷类和二苯乙烯苷类。结论:基于UPLC-Q-TOF-MS/MS技术,快捷、准确、较全面地分析鉴定亚大黄的正丁醇抗补体活性部位的化学成分主要为蒽醌苷和二苯乙烯苷类,为一步分离及开发亚大黄中苷类抗补体活性成分提供科学依据。 Objective:To rapidly analyze the anti-complement active constituents in the Rheum ihasaenseby UPLC-Q-TOF-MS/MS technology,and to provide a reference for elucidating the anti-complement activity pharmacological basis of the rhubarb.Method:95% ethanol extract of rhubarb was extracted to obtain petroleum ether,ethyl acetate and n-butanol.The anti-complement hemolytic activity(CH50) of three parts was determined.UPLC-Q-TOF-MS/MS was used to characterize the chemical constituents of the three parts by using the target compound screening method in the mass spectrometry software,and the chemical composition was identified by the retention time,the exact molecular weight and the secondary mass spectrometry.Result:The values of anticomplement activity of adipsoin was 0.032·mL^-1,which was stronger than that of positive drug heparin.In the optimized LC-MS,the scifinder database,reference substance and related literature werecombined to identify compounds.The main components of petroleum ether were identified,which were mainly fatty acids and sterols.Thirteencompounds from ethyl acetate were identified,mainly free anthraquinones and stilbenes.The main components of n-butanol were identified as mainly anthraquinone glycosides and stilbene glycosides.Conclusion:Based on UPLC-Q-TOF-MS/MS technology,the chemical constituents of the n-butanol-resistant part of the reaction group were mainly anthraquinone and stilbene glycosides,which provided foundation for furtherseparation and development of anti-complement active ingredients from rhubarb.
作者 詹艳芝 吴蓓 黄文平 徐旭 张晶 陈思思 冯育林 杨世林 温泉 ZHAN Yan-zhi;WU Bei;HUANG Wen-ping;XU Xu;ZHANG Jin;CHEN Si-si;FENG Yu-lin;YANG Shi-lin;WEN Quan(National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine, Jiangxi University of Traditional Chinese Medicine, Nanehang 330006, China;Nanchang Food and Drug Inspectio Office, Nanchang 330029, China)
出处 《中国实验方剂学杂志》 CAS CSCD 北大核心 2018年第10期60-66,共7页 Chinese Journal of Experimental Traditional Medical Formulae
基金 江西省卫计委中医药科研项目(2017A291) 国家自然科学青年基金项目(81603274)
关键词 亚大黄 化学成分 抗补体 超高液相色谱四级杆飞行时间质谱 清热解毒 Rheum ihasaense chemical composition anti-complement UPLC-Q-TOF-MS/MS clearing heat and detoxicating
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