摘要
以薯蓣皂苷为原料,1,6-己二异氰酸酯作为间隔臂,采用"一锅法",制备得到一种新型高效液相色谱填料——薯蓣皂苷键合硅胶固定相。通过固体核磁共振技术、红外光谱分析、元素分析、热重分析和电镜扫描等手段对自制的薯蓣皂苷键合硅胶固定相进行结构表征,确证薯蓣皂苷已键合至硅胶表面。采用该固定相,乙腈-水为流动相梯度洗脱,建立三七总皂苷原料药HPLC指纹图谱。以天然产物药用成分制备高效液相色谱填料,为液相色谱固定相制备提供新的思路,也为天然产物中有效成分的分离分析提供了新的途径。
A new stationary phase for HPLC was prepared by one-pot reaction method,using natural active ingredient dioscin as raw material and 1,6-diisocyanate as spacer arm. The structure of new stationary phase was characterized by solid-state NMR techniques,infrared spectroscopy,elemental analysis,thermogravimetric analysis and scanning electron microscope（ SEM）. The results confirmed that dioscin had been immobilized onto the surface of silica gel successfully with suitable thermostability and chemical resistance. The resulting stationary phase contained 127. 6 μmol / g dioscin ligand.The chromatographic performance of the new stationary phase were evaluated using different kinds of solute probes,including non-polar compounds,alkaline compounds and acid compounds. The results showed that the new stationary phase had a typical reversed phase chromatographic property,meanwhile it can provide various interactions with solutes,such as hydrogen bonding,dipole-dipole,π-π etc. It was good on the separation of multi-component natural products. The HPLC fingerprint of PNS（ Panax notoginseng saponins） API（ Active Pharmaceutical Ingredient） on the dioscin-bonded silica gel stationary phase was established. The mobile phase consisted of acetonitrile and water. The results provided technologic support for the quality control of PNS products. It was a new thinking for preparing stationary phase with natural active ingredient and separation complex ingredient in natural products.
出处
《天然产物研究与开发》
CAS
CSCD
北大核心
2015年第5期780-784,共5页
Natural Product Research and Development
基金
国家自然科学基金(81102408)
