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高效液相色谱-二极管阵列检测-离子阱-飞行时间质谱法对龙血通络胶囊中酚类衍生物的表征及定量分析

Characterization and quantitative analysis of phenolic derivatives in Longxuetongluo Capsule by HPLC-DAD-IT-TOF-MS.

作者信息

Sun Jing, Song Yuelin, Sun Hui, Liu Wenjing, Zhang Yunfeng, Zheng Jiao, Zhang Qian, Zhao Yunfang, Xiao Wei, Tu Pengfei, Li Jun

机构信息

Modern Research Center for Traditional Chinese Medicine, School of Chinese Materia Medica, Beijing University of Chinese Medicine, Beijing 100029, China.

National Key Laboratory of Pharmaceutical New Technology for Chinese Medicine, Jiangsu Kanion Pharmaceutical Co. Ltd., Lianyungang 222001, China.

出版信息

J Pharm Biomed Anal. 2017 Oct 25;145:462-472. doi: 10.1016/j.jpba.2017.07.012. Epub 2017 Jul 14.

Abstract

Longxuetongluo Capsule (LTC), which is derived from the total phenolic extract of Chinese dragon's blood, has been proved to be safe as well as effective towards ischemic stroke. However, the effective material basis remains unclear. The present study thereby focused on the clarification of the qualitative and quantitative properties for the phenolic derivatives in LTC. Regarding homolog-focused chemical profiling, the mass fragmentation patterns of the primary subtypes of phenolic compounds such as homoisoflavanones, flavanes, chalcones, and flavonoid oligomers were summarized by assaying authentic references with hybrid ion trap time-of-flight mass spectrometry, and the chemical structures of 124 phenolic compounds, in total, were unambiguously or tentatively annotated in LTC by matching the accurate mass spectral profiles with the proposed mass cracking rules and those reference substances. Afterwards, simultaneous determination of 12 primary phenolic compounds was carried out in different batches of LTC using HPLC-DAD, after that the method was proved to be accurate, precise, and reproducible according to diverse method validation assays. The obtained findings are expected to be meaningful for clarifying the effective substances and quality assessment of LTC.

摘要

龙血通络胶囊(LTC)源自中药血竭的总酚提取物,已被证明对缺血性中风安全有效。然而,其有效物质基础仍不清楚。因此,本研究着重于阐明LTC中酚类衍生物的定性和定量特性。关于以同系物为重点的化学图谱分析,通过用混合离子阱飞行时间质谱法测定标准品,总结了酚类化合物主要亚型如高异黄酮、黄烷、查耳酮和黄酮类低聚物的质谱裂解模式,并通过将精确质谱图与提出的质谱裂解规则及标准物质相匹配,在LTC中明确或初步注释了总共124种酚类化合物的化学结构。之后,采用高效液相色谱-二极管阵列检测法(HPLC-DAD)对不同批次的LTC中12种主要酚类化合物进行了同时测定,经多种方法验证试验证明该方法准确、精密且可重现。所得结果有望对阐明LTC的有效物质和质量评估具有重要意义。

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