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| Study on the preparation process of ginkgolide K |
| 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 |
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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.
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