首页|基于UPLC-Q/TOF-MS和UPLC-QQQ-MS/MS的血栓心脉宁片和胶囊质量分析

基于UPLC-Q/TOF-MS和UPLC-QQQ-MS/MS的血栓心脉宁片和胶囊质量分析

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血栓心脉宁片和胶囊是处方相同、制法不同但功能主治相同的 2 种中成药制剂,具有益气活血,开窍止痛的功效。该研究首次采用UPLC-Q/TOF-MS对血栓心脉宁胶囊进行定性分析,从中鉴定出 61 个化合物,其中酚酸类 9 个、蟾蜍甾类 10个、皂苷类 15 个、胆汁酸类 5 个以及其他类 22 个,与血栓心脉宁片相比,两者化学成分种类略有差异。在此基础上,通过网络药理学研究,构建成分-靶点-通路网络,明确血栓心脉宁治疗冠心病、心绞痛、缺血性脑卒中的活性成分 36 个及共有靶点 31个。针对效毒一体的蟾蜍甾类成分,采用UPLC-QQQ-MS/MS技术建立了其中日蟾毒它灵、沙蟾毒精、蟾毒它灵、蟾毒灵、华蟾酥毒基和脂蟾毒配基的含量测定方法,方法学验证结果表明精密度、稳定性、重复性均符合定量分析要求,6 个待测成分的平均加样回收率依次为 80。84%、98。65%、104。6%、102。7%、83。46%、104。9%。10 批血栓心脉宁片中 6 个成分的质量分数分别为4。13~10。3、20。6~57。9、11。0~32。2、9。52~22。7、1。64~3。39、11。3~19。5 μg·g-1;15 批血栓心脉宁胶囊中6 个成分的质量分数分别为 0。647~5。36、2。69~72。1、2。05~17。6、2。14~24。2、1。19~7。58、2。71~21。8 μg·g-1。结果提示不同剂型、不同厂家、不同批次样品中6 个成分的含量均存在一定的差异。该研究明确了血栓心脉宁片和胶囊的化学成分组成,并通过网络药理学方法预测了其治疗冠心病、心绞痛和缺血性脑卒中的活性成分以及共有靶点和信号通路,为明确其药效物质奠定了基础,同时为完善两者的质量标准、提升质量控制水平提供了检测方法,建议在生产过程中关注血栓心脉宁的投料原料蟾酥的质量。
Quality analysis of Xueshuan Xinmaining Tablets and Capsules based on UPLC-Q/TOF-MS and UPLC-QQQ-MS/MS
Xueshuan Xinmaining Tablets and Capsules are two Chinese patent medicines with the same prescription,different preparation methods but the same function of replenishing Qi,activating blood,opening orifices,and relieving pain.Xueshuan Xinmaining Capsules were qualitatively analyzed by UPLC-Q/TOF-MS for the first time,and 61 compounds were identified,including 9 phenolic acids,10 bufadienolides,15 saponins,5 bile acids,and 22 other compounds.The chemical composition was slightly different between Xueshuan Xinmaining Tablets and Capsules.On this basis,network pharmacology was employed to construct the component-target-pathway network,which clarified 36 active ingredients and 31 common targets of the tablets and capsules for treating coronary heart disease,angina pectoris,and ischemic stroke.A method was developed based on UPLC-QQQ-MS/MS for determining the content of bufadienolides including gamabufotalin,arenobufagin,bufotaline,bufalin,cinobufagin,and resibufogenin.The average recoveries of the six components were 80.84%,98.65%,104.6%,102.7%,83.46%,and 104.9%,respectively.The content of the six components was 4.13-10.3,20.6-57.9,11.0-32.2,9.52-22.7,1.64-3.39,and 11.3-19.5 μg·g-1 in 10 batches of Xueshuan Xinmaining Tablets and 0.647-5.36,2.69-72.1,2.05-17.6,2.14-24.2,1.19-7.58,and 2.71-21.8 μg·g-1 in 15 batches of Xueshuan Xinmaining Capsules,respectively.The results showed that the content of six components varied in the samples of different dosage forms,different manufacturers,and different batches.This study clarified the chemical composition of Xueshuan Xinmaining Tablets and Capsules and predicted the active ingredients,common targets,and signaling pathways for the treatment of coronary heart disease,angina pectoris,and ischemic stroke by network pharmacological methods.The findings laid a foundation for clarifying the pharmacodynamic substances and provided testing methods for improving the quality standards and quality control of Xueshuan Xinmaining Tablets and Capsules.It is recommended that attention should be paid to the quality of toad venom in the production process of Xueshuan Xinmaining Tablets and Capsules.

Xueshuan Xinmaining TabletsXueshuan Xinmaining Capsulesnetwork pharmacologybufadienolidesUPLC-Q/TOF-MSUPLC-QQQ-MS/MS

刘雅婷、纪亮、陈两绵、谢天择、刘晓谦、王智民、刘传贵、朱继忠、高慧敏

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天津中医药大学,天津 301617

中国中医科学院 中药研究所,中药质量控制技术国家工程实验室,北京 100700

吉林华康药业股份有限公司,吉林 敦化 133700

血栓心脉宁片 血栓心脉宁胶囊 网络药理学 蟾蜍甾 UPLC-Q/TOF-MS UPLC-QQQ-MS/MS

中国中医科学院科技创新工程项目中国中医科学院科技创新工程项目中国中医科学院科技创新工程项目国家重点研发计划项目国家药典委员会国家药品标准提高任务项目

CI2021A04002CI2021A05053CI2021A044012023YFC35040002023Z059

2024

中国中药杂志
中国药学会

中国中药杂志

CSTPCD北大核心
影响因子:1.718
ISSN:1001-5302
年,卷(期):2024.49(19)