中国中药杂志

2021, v.46(01) 130-138

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蛇胆中胆汁酸类化学成分分析
Bile acid derivatives-focused chemical profiling in snake bile

曹妍;李婷;常安琪;蒋珍珍;于娟;屠鹏飞;宋月林;
CAO Yan;LI Ting;CHANG An-qi;JIANG Zhen-zhen;YU Juan;TU Peng-fei;SONG Yue-lin;Modern Research Center for Traditional Chinese Medicine, School of Chinese Materia Medica, Beijing University of Chinese Medicine;Zhangzhou Pianzaihuang Parmaceutical Co., Ltd.;

摘要(Abstract):

蛇胆作为传统的名贵中药广泛应用于多种名优中成药的制备,胆汁酸为其主要活性成分。阐明蛇胆中的胆酸类成分,对于建立完整的蛇胆质量控制方法和阐明药效物质均具有重要意义。该文首先利用~1H-NMR技术对蛇胆提取物非靶标性检测,再利用自动馏分接收器剔除蛇胆中的牛磺胆酸部分,收集目标成分,浓缩处理后利用LC-MS对其中的胆酸类成分深入分析。非靶标检测结果表明胆汁酸为蛇胆的主要成分,结合文献及对照品比对,从蛇胆~1H-NMR图谱中初步归属了6个胆酸类成分,分别为鹅去氧胆酸、胆酸、牛磺鹅去氧胆酸、牛磺胆酸、牛磺去氧胆酸和甘氨胆酸。由于其中牛磺胆酸含量过高从而影响微量成分的检出,通过自动接收器剔除蛇胆中的牛磺胆酸后,将处理过的蛇胆提取物经LC-MS平台检测,通过多级质谱数据分析,保留时间匹配,并结合对照品及数据库搜索,共发现并鉴定了57个胆酸类成分。该文基于~1H-NMR和LC-MS平台并半制备蛇胆化学成分对蛇胆中胆酸类成分进行了全面、系统地表征,对蛇胆的质量控制和评价方法的建立具有一定的参考价值。
As a precious traditional Chinese medicine(TCM), snake bile has been widely used in numerous Chinese medicine prescriptions. Bile acid(BA) derivatives have been demonstrated as the primary chemical family in snake bile. In-depth chemical characterization of BAs is of great importance towards the establishment of quality standards and clarification of the effective material basis for snake bile. This study firstly employed ~1H-NMR to preliminarily analyze the chemical profiles of snake bile, an automated fraction collector was subsequently implemented to obtain the fractions-of-interest. The fraction was then concentrated and re-analyzed by LC-MS. Based on ~1H-NMR, BAs were found to be the main components of snake bile, and six BAs including CDCA, CA, TCDCA, TCA, TDCA and GCA were tentatively identified from the representative spectrum with the assistance of literature and reference compounds. Whereas the content of TCA in snake bile was too great, resulting in a great obstacle for the detection of trace components, the automated fraction collector was subsequently implemented to obtain the fractions-of-interest for LC-MS analysis. According to matching MS/MS information and retention time with reference compounds as well as database retrieval, a total of 57 BAs were detected and annotated. Because of the combination of ~1H-NMR and LC-MS platforms, the findings are beneficial for the in-depth characterization of BAs in snake bile, which provides references for the establishment of quality control and evaluation methods of snake bile.

关键词(KeyWords): 蛇胆;胆汁酸;~1H-NMR;自动流分接收器;LC-MS
snake bile;bile acid;~1H-NMR;automated fraction collector;LC-MS

Abstract:

Keywords:

基金项目(Foundation): 国家自然科学基金项目(81773875);; 中国科协青年人才托举工程项目(2017QNRC001)

作者(Author): 曹妍;李婷;常安琪;蒋珍珍;于娟;屠鹏飞;宋月林;
CAO Yan;LI Ting;CHANG An-qi;JIANG Zhen-zhen;YU Juan;TU Peng-fei;SONG Yue-lin;Modern Research Center for Traditional Chinese Medicine, School of Chinese Materia Medica, Beijing University of Chinese Medicine;Zhangzhou Pianzaihuang Parmaceutical Co., Ltd.;

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DOI: 10.19540/j.cnki.cjcmm.20200628.204

参考文献(References):

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