正相高效液相色谱法制备银杏内酯A和银杏内酯B

Preparation of Ginkgolides A and B by Normal-Phase High Performance Liquid Chromatography

以实验室自制的银杏浸膏精制物为原料,采用正相高效液相色谱法分离制备得到银杏内酯A、银杏内酯B 单体．采用φ40mm×300 mm正相色谱柱、蒸发光散射检测器等组成的制备色谱系统,以乙酸乙酯、石油醚和甲醇 混合溶剂作为流动相,通过考察流动相中溶剂配比、流速和上样量等因素对分离效果的影响,确定了适宜的色谱条 件:流动相中乙酸乙酯、石油醚和甲醇的体积比为55:40:5、流速26mL／min、上样量120mg．经过一次分离即可得 到银杏内酯A、B单体,纯度可达99．7％和98．4％,收率分别为73.8％和74．2％．采用IR、13C-NMR、1H-NMR及质谱 进行结构鉴定,结构数据与文献值相符．

This research explores methods to biloba extract （GBE, EGb 761 ） by means separate individual ginkgolides A and B from the enriched ginkgo of normal-phase high-performance liquid chromatography （NPHPLC）. The chromatographic system consisted mainly of a Ф 40 mm × 300 mm column packed with silica gel and an evaporative light scattering detector. The influence of factors, such as the solvent composition, the flow rate of mobile phase and the sample load, on separation efficiency was studied to determine the suitable eluting condition. The results were as follows ： the mobile phase was the mixed solvent of ethyl acetate-petroleum ethermethanol with volumetric ratio of 55： 40： 5. 120 mg sample was eluted at the flow rate of 26 mL/min. With one separation process ginkgolides A and B monomer with the purity of 99.7% and 98.4% and yields of 73.8% and 74.2% were obtained respectively. The structure identification results by IR, ^13 C-NMR, ^1H-NMR and MS showed good agreement with those in literature.