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首页> 外文期刊>Rapid Communications in Mass Spectrometry: RCM >Characterization of isoquinoline alkaloids, diterpenoids and steroids in the Chinese herb Jin-Guo-Lan (Tinospora sagittata and Tinospora capillipes) by high-performance liquid chromatography/electrospray ionization with multistage mass spectrometry
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Characterization of isoquinoline alkaloids, diterpenoids and steroids in the Chinese herb Jin-Guo-Lan (Tinospora sagittata and Tinospora capillipes) by high-performance liquid chromatography/electrospray ionization with multistage mass spectrometry

机译：高效液相色谱/电喷雾电离多级质谱法表征中药材金国兰（Tinospora sagittata和Tinospora capillipes）中的异喹啉类生物碱，二萜类化合物和类固醇

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This study sought to determine the primary components (isoquinoline alkaloids, diterpenoids and steroids) in crude extracts of the Chinese herb Jin-Guo-Lan, prepared from the roots of Tinospora sagittata and T. capillipes, by liquid chromatography/electrospray ionization multistage mass spectrometry coupled with diode-array detection (LC-DAD/ESI-MSn). After separation on a reversed-phase C-18 column using gradient elution, positive and negative ESI-MS experiments were performed. In positive ion mode, the three types of compounds showed very different characteristic ions: strong [M](+) or [M+H](+) ions were observed for isoquinoline alkaloids; [M+NH4](+) and/or [M+H-CO2](+) for diterpenoids; [M+H-nH(2)O](+) (n=1-3) for steroids. These adduct ions and/or fragments were used to deduce the mass and categories of known and unknown component's in crude extracts, and their structures were further confirmed by ESI-MSn in positive ion mode. Moreover, UV absorption peaks obtained from DAD provided useful functional group information to aid the MSn-based identification. As a result, 11 compounds were unambiguously identified by comparing with standard compounds and 13 compounds were tentatively identified or deduced according to their MSn data. Two of these compounds (13-hydroxycolumbamine and 13-hydroxyjatrorrhizine) were found to be new compounds and another one (13-hydroxypalmatine) was detected for the first time as a natural product. In addition, a [M-CH3-H2O](+) ion in MS2 of [M](+) after insource collision-induced dissociation was used to differentiate positional isomers of protoberberine alkaloids, columbamine and jatrorrhizine. Although the roots of T. sagittata and T. capillipes contain almost identical compounds, the content of the compounds in them is dramatically different, suggesting the necessity for further comparison of the bioactivities of the two species. Copyright (c) 2006 John Wiley & Sons, Ltd.
机译：这项研究试图通过液相色谱/电喷雾电离多级质谱法测定从箭果和毛冠线虫的根中提取的中草药金国兰粗提物中的主要成分（异喹啉类生物碱，二萜和类固醇）。结合二极管阵列检测（LC-DAD / ESI-MSn）。在使用梯度洗脱的反相C-18色谱柱上分离后，进行了正和负ESI-MS实验。在正离子模式下，这三种类型的化合物显示出非常不同的特征离子：异喹啉生物碱中观察到强[M]（+）或[M + H]（+）离子;二萜类化合物为[M + NH4]（+）和/或[M + H-CO2]（+）;类固醇的[M + H-nH（2）O]（+）（n = 1-3）。这些加合物离子和/或碎片用于推导粗提物中已知和未知成分的质量和类别，并通过ESI-MSn在正离子模式下进一步证实其结构。此外，从DAD获得的UV吸收峰提供了有用的官能团信息，有助于基于MSn的鉴定。结果，通过与标准化合物的比较明确鉴定出11种化合物，并根据其MSn数据初步鉴定或推导了13种化合物。这些化合物中的两种（13-羟基哥伦巴胺和13-羟基麻疯子碱）被发现是新化合物，另一种化合物（13-羟基巴马汀）是首次作为天然产物被检测到。此外，在源碰撞碰撞解离后，[M]（+）的MS2中的[M-CH3-H2O]（+）离子用于区分原小ber碱生物碱，哥伦巴胺和麻疯子碱的位置异构体。尽管箭毛和毛鳞茎的根中含有几乎相同的化合物，但它们中化合物的含量却截然不同，这表明有必要进一步比较这两个物种的生物活性。版权所有（c）2006 John Wiley＆Sons，Ltd.

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