银杏内酯提取物中微量成分的LC/DAD/ESI/MS分析及结构鉴定

目的　银杏内酯提取物中有关微量成分的鉴别。方法　采用LC DAD ESI MS联用技术。结果　鉴别了已知的银杏内酯A ,B ,C ,J,M以及白果内酯,并发现了3个微量未知化合物。结论　根据UV ,IR ,MS和NMR光谱数据,鉴定了其中两个新化合物的结构,分别为1,10-二羟基-3,14-二去氢银杏内酯和10-羟基3,14-二去氢银杏内酯,并命名为GK和GL。

ANALYSIS AND STRUCTURE IDENTIFICATION OF TRACE CONSTITUENT IN THE TOTAL GINKGOLIDE BY USING LC/DAD/ESI/MS

AIM To identify the trace constituents in the total ginkgolide from leaves of Ginkgo biloba . METHODS The extract was analyzed by using LC/DAD/ESI/MS combination technology, both UV and mass spectrums of each compound were recorded simultaneously. UV, IR, MS and NMR spectra were employed for structural identification. RESULTS With higher sensitivity of the MS detector, three trace constituents were found as well as the known compounds ginkgolide A (GA), ginkgolide B (GB), ginkgolide C (GC) and bilobalide (BD). CONCLUSION Two compounds ( t R 57 8 and 56 7 min) were identified as 1,10 dihydroxy 3,14 didehydroginkgolide and 10 hydroxy 3,14 didehydroginkgolide, named as ginkgolide K and ginkgolide L, respectively, according to the characteristics of their UV, MS, IR and NMR spectra. It is the first time of finding the ginkgolide compounds containing double bond.