摘要
目的:建立枸杞子多糖柱前衍生HPLC指纹图谱。方法:以三氟乙酸(TFA)水解枸杞子多糖,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测定枸杞子多糖中单糖的衍生物。采用ZORBAX Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm),流动相0.1 mol·L-1磷酸缓冲液(p H 6.7)-乙腈(84.5∶15.5),流速0.8 m L·min-1,检测波长250 nm,柱温30℃。结果:枸杞子多糖柱前衍生指纹图谱标示出11个共有峰,鉴别了8个共有峰(D-甘露糖,L-鼠李糖,D-葡萄糖醛酸,D-半乳糖醛酸,D-葡萄糖,D-半乳糖,D-木糖,D-阿拉伯糖)。10批枸杞子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,可有效控制枸杞子多糖的质量。
Objective： The aim of this study was to establish a pre-column derivation HPLC method for chromatographic fingerprint of Lycii Fructus Polysaccharide. Method： Lycii Fructus sample was hydrolyzed with Trifluoroacetic Acid（ TFA） and derivated by 1-phenyl-3-methyl-5-pyrazolone（ PMP）. The monosaccharide composition of Lycii Fructus polysaccharide was carried out by reversed-phase technique on a ZORBAX Eclipse XDB-C18 column with a mobile phase composed of 0. 1 mol·L^-1phosphate buffer（ p H 6. 7） and acetonitrile in the ratio of 84. 5∶ 15. 5. The flow rate was set at 0. 8 m L·min^-1,the wavelength was set at 250 nm,and the column temperature was at 30 ℃. Result： There were 12 peaks from the fingerprint and 8 peaks were D-Man,L-Rha,D-Glc UA,D-Glc N, D-Glc, D-Gal, D-Xyl, D-Ara. The similarity of the 10 batches of Lycium barbarum samples was more than 0. 99. Conclusion： The HPLC method with pre-column derivatization is appropriate for the analysis of monosaccharide composition of Lycii Fructus polysaccharide and the method is simple,quick and accurate.
出处
《中国实验方剂学杂志》
CAS
北大核心
2014年第22期53-56,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
广东省部产学研结合项目(2012B090600025)
关键词
枸杞子
多糖
柱前衍生化
高效液相色谱
指纹图谱
Lycii Fructus
polysaccharide
pre-column derivatives
monosaccharide
HPLC
fingerprint chromatogram
作者简介
蒋梅，硕士，从事创新中药与指纹图谱分析研究，Tel：020—39358519，E-mail：Jamie125@163．com
[通讯作者]魏刚，研究员，博士生导师，从事创新中药与指纹图谱分析研究，Tel：020—39358166，E-mail：weigang21@163．com
