首页|基于PMP柱前衍生化-HPLC法的淫羊藿多糖的单糖指纹图谱研究

基于PMP柱前衍生化-HPLC法的淫羊藿多糖的单糖指纹图谱研究

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建立了淫羊藿多糖酸水解的柱前衍生化单糖HPLC指纹图谱方法.淫羊藿多糖经2.0mol/L盐酸水解,再经1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化处理后,用HPLC法测定其单糖组成.采用YMC-Pack ODS-A柱(4.6 mm×250 mm,5 μm),以磷酸盐缓冲液-乙腈为流动相,流速为0.8 mL/min,检测波长为254nm.采用2012年版《中药色谱指纹图谱相似度评价系统》,建立了 40批淫羊藿样品的共有指纹图谱,确立了10个共有峰,通过与对照品比对,指认了8个共有峰,分别为D-甘露糖、D-葡萄糖醛酸、鼠李糖、半乳糖醛酸、D-无水葡萄糖、半乳糖、木糖和阿拉伯糖.通过相似度结合正交偏最小二乘法,对7批巫山淫羊藿进行分析.结果显示,相似度小于0.9,并得到4个差异性单糖成分.建立的指纹图谱方法简单、易操作,可为淫羊藿药材的质量评价提供参考.
Monosaccharide Fingerprint of Epimedium Polysaccharides Based on PMP Pre-column Derivatization and HPLC Method
The monosaccharide HPLC fingerprint method of Epimedium polysaccharides using acid hydrolysis by pre-column derivatization was established.The Epimedium polysaccharides were hydrolyzed into monosaccharides by 2.0 mol/L hydrochloric acid and derivatized by 1-phenyl-3-methyl-5-pyrazolone(PMP).Then,the monosaccharide components were detected by HPLC.The YMC-Pack ODS-A column(4.6 mm×250 mm,5 μm)was used with a mixture of phosphate buffer and acetonitrile as the mobile phase,in a flow rate of 0.8 mL/min and at a detection wavelength of 254 nm.The common fingerprints of forty batches of Epimedii Folium were established with ten common peaks by Similarity Evaluation System for Chromatographic Fingerprint of TCM(Version 2012).Eight peaks in which were identified as D-mannose,D-glucuronic acid,rhamnose,galacturonic acid,D-glucose,galactose,xylose and arabinose by reference substances.Similarity analysis and orthogonal partial least squares analysis were applied to investigate the differences between Epimedium and seven batches of E.wushanense T.S.Ying.The similarities were less than 0.9,and four monosaccharides showing significant differences were distinguished.The established method is simple and repeatable,which can provide references for the quality evaluation of Epimedium.

Epimedii Foliumpolysaccharidemonosaccharidepre-column derivatizationHPLCfingerprint

黄春跃、杨子璇、孙宜春、李慧馨、胡晓

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中国医药工业研究总院有限公司,上海医药工业研究院有限公司,先导物成药性研究全国重点实验室,上海 201203

国药集团同济堂(贵州)制药有限公司,贵州贵阳 550009

淫羊藿 多糖 单糖 柱前衍生化 HPLC 指纹图谱

国家自然科学基金上海市自然科学基金中央引导地方科技发展资金项目

3227042121ZR1461800GZIM 202001-9-2

2024

中国医药工业杂志
上海医药工业研究院,中国化学制药工业协会

中国医药工业杂志

CSTPCD
影响因子:0.487
ISSN:1001-8255
年,卷(期):2024.55(1)
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