A rapid and simple determination of protoberberine alkaloids in Rhizoma Coptidis by 1H NMR and its application for quality control of commercial prescriptions
A rapid and simple determination of protoberberine alkaloids in Rhizoma Coptidis by 1H NMR and its application for quality control of commercial prescriptions
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DOI：
10.1016/j.jpba.2009.02.028
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发表时间：
2009-07-12
影响因子：
3.4
通讯作者：
Wu, Tian-Shung
中科院分区：
文献类型：
--
作者：
Li, Chia-Ying;Tsai, Sung-I.;Wu, Tian-Shung
大黄是具有重要生物活性的中草药，其生物碱成分的分析需要简便、灵敏、准确的分析方法。建立了一种高特异性、高灵敏度的1H-1 NMR测定黄连属植物及其商品方剂中原小檗碱类生物碱小檗碱、巴马汀、黄连碱和药根碱的方法。对目标原小檗碱生物碱的H-13信号进行H-1 NMR分析。通过比较不同溶剂对信号分辨的影响，选择了甲醇-d（4）-苯-d（6），（75：25）为最佳溶剂。通过各化合物目标峰的积分值与内标蒽已知量的相对比值计算化合物的量。该方法可在5 min内快速、简便地定量黄连中的原小檗碱生物碱，且无需任何预纯化步骤。黄连中生物碱的回收率在93- 105%之间。该方法的优点是校准曲线不需要参考化合物，可以直接在粗提取物上实现定量，并且与常规HPLC方法相比，可以实现对原小檗碱生物碱的更好的选择性和非常显著的时间增益。皇冠版权所有（C）2009年出版的爱思唯尔B. V.保留所有权利。
Simple, convenient, sensitive and accurate analytical methods are needed for the analysis of alkaloid components in Rhizoma Coptidis in traditional Chinese herbal medicine, which has important bioactivity. In the present study, a highly specific and sensitive method using H-1 NMR has been developed for the quantitative determination of protoberberine alkaloids berberine, palmatine, coptisine and jatrorrhizine in Coptis species and their commercial traditional Chinese medicine prescriptions. A H-1 NMR analysis of the H-13 signals of target protoberberine alkaloids was performed. By comparing the solvent effects on the resolution of these signals, methanol-d(4)-benzene-d(6), (75:25) is selected as an optimal H-1 NMR solvent. The quantity of the compounds is calculated by the relative ratio of the integral values of the target peak for each compound to the known amount of the internal standard anthracene. This method allows rapid and simple quantitation of protoberberine alkaloids from Coptis species and the more complex commercial prescriptions in 5 min without any pre-purification steps. The recoveries of these alkaloids from Coptis chinensis are in the range of 93-105%. Limit of detection of berberine in the plant material or prescription is 0.03 mg/mL The advantages of this method are that no reference compounds are required for calibration curves, the quantification can be directly realized on a crude extract, and the better selectivity for protoberberine alkaloids and a very significant time-gain can be achieved, in comparison to conventional HPLC methods, for instance. Crown Copyright (C) 2009 Published by Elsevier B.V. All rights reserved.