Pharmazeutisches Institut, Abteilung Pharmazeutische Biologie, Christian-Albrechts-Universität zu Kiel, Gutenbergstraße 76, 24118, Kiel, Germany.
Pharmazeutisches Institut, Abteilung Pharmazeutische und Medizinische Chemie, Christian-Albrechts-Universität zu Kiel, Gutenbergstraße 76, 24118, Kiel, Germany.
J Pharm Biomed Anal. 2018 Jun 5;155:109-115. doi: 10.1016/j.jpba.2018.03.056. Epub 2018 Mar 30.
Quantitative analysis is an important field in the quality control of medicinal plants, aiming to determine the amount of pharmacologically active constituents in complex matrices. Often biological effects of herbal drugs are not restricted to single compounds, but are rather caused by a number of often biogenetically related plant metabolites. Depending on the complexity of the analyzed plant extract, conflicts between accuracy, such as total content assays using photometric or colorimetric methods, and comprehensiveness, e.g. quantification of one or a few lead compounds can occur. In this study, we present a qHNMR approach determining the total amount of cycloartanoids in black cohosh (Actaea racemosa) rhizomes. Perdeuterated methanol containing 1,2,4,5-tetrachloro-3-nitrobenzene as an internal standard was used for extraction. Amounts of cycloartanoids were then measured by integrating H NMR signals of all cycloartenoids' H-19 exo protons. Due to their unusually low chemical shifts, these signals are well separated from all remaining signals in crude extracts. Thus, accurate (recovery rates of 99.5-102.5%) and precise (relative standard deviations below 2.5%) quantification of cycloartanoids was accomplished. To the best of our knowledge, this is the first example of a quantification of the total amount of a pharmacologically relevant compound class by integration of one H NMR signal characteristic for all members of this particular compound class. Additionally, we propose a new term and unit for the evaluation of medicinal plants and herbal medicinal products: the "specific partial amount of substance" of pharmacologically active constituents, indicated in mmol/g.
定量分析是药用植物质量控制的一个重要领域，旨在确定复杂基质中具有药理活性的成分的含量。草药的生物效应通常不限于单一化合物，而是由许多通常具有生物相关性的植物代谢物共同作用引起的。根据分析植物提取物的复杂程度，准确性（例如使用分光光度法或比色法测定总含量）和全面性（例如，定量测定一种或几种先导化合物）之间可能会发生冲突。在本研究中，我们提出了一种 qHNMR 方法，用于测定黑升麻（Actaea racemosa）根茎中环阿尔廷烷类化合物的总量。使用含有 1,2,4,5-四氯-3-硝基苯作为内标物的氘代甲醇进行提取。然后通过整合所有环阿尔廷烷类化合物 H-19 外向质子的 H NMR 信号来测量环阿尔廷烷类化合物的含量。由于它们的化学位移异常低，这些信号与粗提物中的所有其他信号完全分离。因此，实现了准确（回收率为 99.5-102.5%）和精确（相对标准偏差低于 2.5%）的环阿尔廷烷类化合物定量。据我们所知，这是首例通过整合所有此类特定化合物成员都具有的一个 H NMR 信号来定量药理学相关化合物类别的总含量的实例。此外，我们提出了一个用于评估药用植物和草药产品的新术语和单位：“具有药理活性成分的特定部分物质含量”，以 mmol/g 表示。
