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通过高效液相色谱(HPLC)、质谱(MS)、核磁共振谱(NMR)等技术详细研究了甘草酸单铵盐原药中主成分及其有关物质的色谱和波谱学特征。本试验通过HPLC对原药主成分及其有关物质进行定位,对欧洲药典7.0版和英国药典2012年版收载的甘草酸单铵盐质量标准中主成分异构体的分离以及对色谱图中相对保留时间约为1.2的化合物的结构归属产生质疑。利用高分辨电喷雾电离质谱(HR-ESI-MS)确定相对分子量和分子式,并计算分子不饱和度;通过COSY、HSQC、NOESY和HMBC二维核磁共振技术,对各物质的1H NMR、13C NMR谱信号进行全归属,获得进一步的结构信息。结果表明,甘草酸单铵盐原药中主成分为18α,20β-甘草酸和18β,20β-甘草酸,有关物质A和相对保留时间约1.2的化合物归属为(18β,20β)-24-羟基-甘草酸和18β,20α-甘草酸。
The chromatographic and spectroscopic characteristics of the main components and their related substances in the monoammonium glycyrrhizinate crude drug were studied in detail by high performance liquid chromatography (HPLC), mass spectrometry (MS) and nuclear magnetic resonance spectroscopy (NMR). In this study, the main components of the original drug and its related substances were located by HPLC. The separation of the main component isomers from the European Pharmacopoeia version 7.0 and British Pharmacopoeia 2012 edition of the mono-ammonium glycyrrhizinate quality standards and the relative Structural assignments of compounds with retention times of about 1.2 were questioned. The relative molecular weights and molecular formulas were determined by high resolution electrospray ionization mass spectrometry (HR-ESI-MS) and the molecular unsaturation was calculated. The 1H NMR, 13C NMR spectra of each material were determined by COZY, HSQC, NOESY and HMBC 2D NMR techniques The spectral signal is fully assigned for further structural information. The results showed that the compounds with 18α, 20β-glycyrrhizic acid and 18β, 20β-glycyrrhizic acid as main components in the glycyrrhizic acid monoammonium salt original substance and the related substance A and the relative retention time of about 1.2 belonged to (18β, 20β) -24-hydroxy Glycyrrhizinic acid and 18β, 20α-glycyrrhizic acid.