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基于定量核磁共振的党参质量评价

Quality assessment of Radix Codonopsis by quantitative nuclear magnetic resonance.

作者信息

Li Chia-Ying, Xu Hong-Xi, Han Quan-Bin, Wu Tian-Shung

机构信息

Department of Applied Chemistry and Life Science, National Pingtung University of Education, Pingtung 900, Taiwan.

出版信息

J Chromatogr A. 2009 Mar 13;1216(11):2124-9. doi: 10.1016/j.chroma.2008.10.080. Epub 2008 Oct 25.

Abstract

Radix Codonopsis (Dangshen) is a famous traditional Chinese medicine and has long been used for replenishing energy deficiency, strengthening the immune system, lowering blood pressure and improving appetite in China, Japan and Korea. A highly specific quantification method using (1)H NMR has been developed for the simultaneous determination of novel quaternary ammonium alkaloids codotubulosine A and B, adenosine and 5-(hydroxymethyl)furfural in Radix Codonopsis materials Codonopsis pilosula, C. pilosula var. modesta, C. tangshen, C. tubulosa, C. subglobosa, C. clematidea, C. lanceolota and Campanumoea javanica collected from different regions of China and Taiwan. A solid-phase extraction with C-18 cartridge followed by elution with water can easily remove sugars the major components that may affect the determination of target constituents. In the (1)H NMR spectrum, the signals of N-CH(3) of codotubulosine A (delta 2.75) and B (delta 2.83), H-8 of adenosine (delta 8.15), and CHO signal of 5-(hydroxymethyl)furfural (delta 9.49) are well separated from other signals in [(2)H(4)]methanol. The quantity of the compounds was calculated by the relative ratio of the integral values of the target peaks of each compound to the known amount of internal standard pyrazine. The described NMR method is found to be relatively simple, specific, precise and accurate for the quality control of Radix Codonopsis herbs and no reference compounds are required for calibration curves, in comparison to conventional HPLC methods, for instance.

摘要

党参是一种著名的传统中药,在中国、日本和韩国长期用于补充气虚、增强免疫系统、降低血压和增进食欲。已开发出一种使用¹H NMR的高特异性定量方法,用于同时测定采自中国不同地区和台湾的党参药材党参、素花党参、川党参、管花党参、球花党参、新疆党参、狭叶党参和鸡蛋参中的新型季铵生物碱党参碱A和B、腺苷和5-(羟甲基)糠醛。用C-18柱进行固相萃取,然后用水洗脱,可以轻松去除可能影响目标成分测定的主要成分糖类。在¹H NMR谱中,党参碱A(δ 2.75)和B(δ 2.83)的N-CH₃信号、腺苷的H-8(δ 8.15)信号以及5-(羟甲基)糠醛的CHO信号(δ 9.49)在[²H₄]甲醇中与其他信号很好地分离。通过各化合物目标峰积分值与已知量内标吡嗪的相对比值计算化合物的含量。与传统的HPLC方法相比,例如,所描述的NMR方法对于党参药材的质量控制相对简单、特异、精密且准确,并且校准曲线无需参考化合物。

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