黄精多糖水解物柱前衍生HPLC指纹图谱

Pre-column Derivatives HPLC Fingerprint of Polygonati Rhizoma Polysaccharide Hydrolysate

目的:建立黄精多糖柱前衍生HPLC指纹图谱。方法:以三氟乙酸(TFA)水解黄精多糖,水解产物加入1-苯基-3-甲基-5-吡唑啉酮(PMP)进行衍生化,采用HPLC测定单糖的衍生物。采用ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×250mm,5μm),流动相0.1 mol·L-1磷酸缓冲液(p H 6.7)-乙腈(84.5∶15.5),检测波长250 nm,柱温30℃,流速0.8 m L·min-1。结果:黄精多糖柱前衍生指纹图谱标示出10个共有峰,鉴别了7个共有峰(D-甘露糖,D-半乳糖醛酸,L-鼠李糖,D-半乳糖,D-葡萄糖,D-木糖,D-阿拉伯糖)。10批黄精药材指纹图谱相似度>0.99。结论:该方法简便,分离度高,重复性及稳定性良好,可有效控制黄精多糖的质量。

Objective： To establish a pre-column derivation HPLC method of chromatographic fingerprint of Polygonati Rhizoma polysaccharide. Method： Polygonati Rhizoma polysaccharide was hydrolyzed with trifluoroacetic acid and derivated by 1-phenyl-3-methyl-5-pyrazolone （PMP）. The monosaccharide composition was separated by reversed-phase technique on a Zorbax Eclipse XDB-Cls column （4. 6 mm ×250mm,5μm） with a mobile phase composed of 0. 1 mol·L^-1 phosphate buffer （pH 6.7） and acetonitrile in the ratio of 84.5 ： 15.5. The flow rate was 0. 8 mL·min-1. The detection wavelength was set at 250 nm, and column temperature was at 30 ℃. Result： There were 10 common peaks from the fingerprint and 7 peaks were identified as D-mannose, L- rhamnose, D-galacturonic, D-galactose, D-glucose, D-xylose, and D-arabinose. The similarity of 10 batches of Polygonati Rhizoma polysaccharide was more than 0.99. Conclusion： The method is accurate and reproducible, which can be used for the quality control of Polygonati Rhizoma.