CUI Long1,2 HU Shaoyin1,2 GAO Jin1,2,3 ZHOU Xiaobo3 SHANG Qiang1,2,3
1.Livzon Pharmaceutical Group Co. Ltd., Guangdong Province, Zhuhai 519090, China;
2.National Engineering Research Center for Modernization of Traditional Chinese Medicine, Guangdong Province, Zhuhai 519090, China;
3.State Key Laboratory of Quality Control of Traditional Chinese Medicine, Macau University of Science and Technology, Macau 999078, China
Abstract：Objective To optimize the preparation process of ginkgolide K. Methods Taking ginkgolide B as raw material, the yield of ginkgolide B as index, the ratio of feed (ginkgolide ∶ diethylaminotrifluoride), the ratio of reaction solvent (ginkgolide ∶ dichloromethane), reaction time and reaction temperature were investigated. The optimum preparation conditions of ginkgolide K were optimized by orthogonal design, and its structure was identified by spectroscopy and the content was detected by high performance liquid chromatography. The high performance liquid chromatography was performed on a ZORBAX SB-C18 chromatography column (250 mm × 4.6 mm, 5 μm) and with the detection wavelength at 220 nm. The mobile phase was water-acetonitrile-isopropyl alcohol (60∶35∶5), flow rate was 1.0 mL/min, column temperature was 30℃. Results The optimum preparation conditions of ginkgolide K were as follows: the feed ratio was 1∶4.5, solvent ratio was 1∶30, reaction time was 20 min and reaction temperature was 4℃. The target compound was identified as ginkgolide K by Q-TOF-MS, 1H-NMR, 13C-NMR and two-dimensional NMR spectroscopy. Conclusion The preparation process is mild, the preparation cycle is short, the operation is simple, the yield is high, and it is suitable for industrial production.
崔龙1,2 胡少银1,2 高进1,2,3 周小波3 尚强1,2,3. 银杏内酯K的制备工艺研究[J]. 中国医药导报, 2019, 16(4): 43-46.
CUI Long1,2 HU Shaoyin1,2 GAO Jin1,2,3 ZHOU Xiaobo3 SHANG Qiang1,2,3. Study on the preparation process of ginkgolide K. 中国医药导报, 2019, 16(4): 43-46.
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2019, Vol. 16 
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