天然产物研究与开发 ›› 2014, Vol. 26 ›› Issue (6): 824-829.

• 研究论文 • 上一篇    下一篇

人参皂苷Rg1键合硅胶固定相的制备、表征及应用(二)

谷晓娟,韩亚琼,李心怡,沈报春*   

  1. 昆明医科大学药学院 云南省天然药物药理重点实验室,昆明 650500
  • 出版日期:2014-06-28 发布日期:2014-11-12

Preparation,Characterization and Application of Ginsenoside Rg1bonded Silica Gel Stationary Phase(Ⅱ)

GU Xiao-juan, HAN Ya-qiong, LI Xin-yi, SHEN Bao-chun*   

  1. School of Pharmaceutical Science & Yunnan Key Laboratory of Pharmacology for Natural Products,Kunming Medical University,Yunnan Kunming 650500 ,China
  • Online:2014-06-28 Published:2014-11-12

摘要: 采用“一锅法”,以1,6-己二异氰酸酯作为间隔臂,制备了一种新型天然中草药药用成分键合固定相——人参皂苷Rg1键合硅胶固定相(250 mm×4.6 mm,5 μm),以元素分析、热重分析和电镜扫描对自制的人参皂苷Rg1键合硅胶固定相进行表征。采用该固定相,建立三七总皂苷原料药的HPLC指纹图谱方法,乙腈-水为流动相梯度洗脱,检测波长203 nm,柱温25 ℃,流速0.8 mL/min,进样量10 μL。以人参皂苷Re色谱峰为参照峰,确定20个共有峰。10批三七总皂苷原料药指纹图谱相似度为0.882~0.999。以人参皂苷Rg1键合硅胶固定相分离三七总皂苷中的皂苷成分,为天然产物的分离分析提供新的思路。

关键词: 高效液相色谱, 指纹图谱, 人参皂苷Rg1键合硅胶固定相, 固定相表征, 三七总皂苷原料药

Abstract: A new ginsenoside Rg1-bonded silica gel stationary phase (250 mm×4.6 mm,5 μm) was prepared by one-pot reaction methodusing 1,6-diisocyanate as spacer arm.The characterization of the new self-made ginsenoside Rg1-bonded silica gel stationary was done by elemental analysis,thermal analysis and scanning electron microscope(SEM).The HPLC fingerprint of Active Pharmaceutical Ingredient (API) of Panax notoginseng saponins (PNS) on the ginsenoside Rg1-bonded silica gel stationary phase was established.The chromatographic fingerprints of 10 batches PNS API were determined on the self-made ginsenoside Rg1-bonded silica gel column.The mobile phase consisted of acetonitrile and water with gradient elution mode.The detection wavelength was 203 nm,the column oven temperature was maintained at 25 ℃,the flow rate was 0.8 mL/min and the injection volume was 10 μL.Based on the peak of ginsenoside Re,20 common peaks were selected,the similarity between 10 batches of samples were within 0.882-0.999.This study provided a new idea for natural products analysis using ginsenoside Rg1-bonded silica gel stationary phase.

Key words: HPLC, fingerprint, ginsenoside Rg1-bonded silica gel stationary phase, characterization of stationary phase, active pharmaceutical ingredient of Panax notoginseng saponins

中图分类号: 

R282 R917 O658