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| Study on preparation of high purity ginkgolide by atmospheric pressure silica gel column chromatography |
| ZHENG Xiangwei1 WU Peiying2 WANG Jun2 WANG Dandan2 RUAN Kefeng1 LIANG Shuang1 FENG Yi1 |
1.Engineering Research Center of Modern Preparation Technology of TCM, Ministry of Education, Shanghai University of Traditional Chinese Medicine, Shanghai 201203, China;
2.SPH Xing Ling Sci.＆Tech. Pharmaceutical Co., Ltd, Shanghai 201703, China |
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Abstract Objective To explore an economical and practical scale preparation technique for high purity ginkgolide (≥80%). Methods Based on the content and transfer rate, the key parameters affecting the chromatographic separation were investigated by single factor, and the optimal technological route of separating and purifying ginkgolide from extract of ginkgo biloba leaves (GBE) was screened out. The total lactones of ginkgo was detected by high performance liquid chromatography (Chinese pharmacopoeia 2010 edition 1 appendix Ⅵ D). Chromatographic conditions included octadecyl silane bonded silica gel being filler, methanol-water (21∶79) being mobile phase, detection by differential refractive index detector, column temperature being at 30℃. The number of theoretical plates should be no less than 2500 according to the peak of bilobalide, ginkgolide A, ginkgolide B and ginkgolide C. Results The results showed that the use of silica gel column chromatography combined with recrystallization process achieved the purpose. The optimal process parameters were as follows: silica gel with particle size of 200-300 mesh, packed column by way of wet method (diameter to diameter ratio 1∶10), loaded sample by way of dry method (loading ratio 1∶50), eluted by means of dichloromethane-methanol (40∶1, 35∶1, V/V) successively, the eluted products were dissolved in acetone-water (1∶1, V/V) and allowed to stand overnight and filter crystallization, so as to obtain the total ginkgolides with the purity of ≥80%, in which the total recovery was 55.4%. Conclusion The process requires simple equipments, large processed capacity, and low production costs. It has industrial production potential.
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