银杏内酯K的制备工艺研究  

Study on the preparation process of ginkgolide K

作　　者：崔龙 胡少银 高进 周小波[3] 尚强 CUI Long;HU Shaoyin;GAO Jin;ZHOU Xiaobo;SHANG Qiang(Livzon Pharmaceutical Group Co.Ltd.,Guangdong Province,Zhuhai 519090,China;National Engineering Research Center for Modernization of Traditional Chinese Medicine,Guangdong Province,Zhuhai 519090,China;State Key Laboratory of Quality Control of Traditional Chinese Medicine,Macao University of Science and Technology,Macao 999078,China)

机构地区：[1]丽珠医药集团股份有限公司,广东珠海519090 [2]国家中药现代化工程技术研究中心,广东珠海519090 [3]澳门科技大学中药质量研究国家重点实验室,澳门999078

出　　处：《中国医药导报》2019年第4期43-46,共4页China Medical Herald

摘　　要：目的优选银杏内酯K的制备工艺。方法以银杏内酯B为原料,以银杏内酯B的收率为指标,考察投料比(银杏内酯∶二乙氨基三氟化硫)、反应溶剂用量比(银杏内酯∶二氯甲烷)、反应时间、反应温度,采用正交试验设计优选银杏内酯K的最佳制备工艺条件,并采用波谱法鉴定其结构,高效液相色谱法测定其含量,色谱条件为:ZORBAX SB-C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:水-甲醇-异丙醇(60∶35∶5);柱温:30℃;流速:1.0 mL/min;检测波长:220 nm。结果银杏内酯K的最佳制备工艺条件为投料比1∶4.5,反应溶剂用量比1∶30,反应时间20 min,反应温度4℃;所得目标化合物经Q-TOF-MS、~1H-NMR、^(13)C-NMR和二维核磁共振谱鉴定为银杏内酯K。结论该制备工艺条件温和、制备周期短、操作简便、收率高,适合工业化生产。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,5μm)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.

关 键 词：银杏内酯 银杏内酯K 氟化试剂 结构鉴定 

分 类 号：R283[医药卫生—中药学]