银杏叶中银杏萜内酯的GC-MS定性定量分析  

Quality and quantity analysis of terpene lactones from Ginkgo biloba leaves by GC-MS

作　　者：唐红芳[1] 郑自强 朱晓雨 毛丽珍[1] 

机构地区：[1]浙江省医学科学院,浙江杭州310013 [2]浙江出入境检验检疫局,浙江杭州310012

出　　处：《中草药》2003年第3期214-217,共4页Chinese Traditional and Herbal Drugs

基　　金：浙江省中医药管理局青年科研基金 ( 1999年 )资助项目;浙江省分析测试基金资助项目 ( 0 0 0 2 1)

摘　　要：目的　建立银杏叶中银杏内酯 A,B,C和白果内酯的定性定量分析方法。方法　银杏叶以 2 0 %乙醇超声提取 ,乙酸乙酯萃取 ,再经酸性氧化铝 -活性炭 -硅藻土混合柱层析 ,在 10 0℃以双 -三甲基硅烷三氟乙酰胺硅烷化 6 0min后 ,用 HP- 5 MS毛细管色谱柱 ,柱温从 180℃程序升温至 30 0℃。采用选择离子监测 ( SIM)方式 ,以峰值最高的碎片离子作为监视离子进行定量分析。结果　银杏内酯 A,B,C和白果内酯的保留时间分别为 13.7,14.3,15 .3和 6 .8min,特征 (监视 )离子 ( m/ z)分别为 5 37,6 2 5 ,713及 45 5 ( 2 99) ;平均回收率分别为 10 2 .0 %,99.4%,96 .0 %和 96 .3%,RSD分别为 0 .5 4%,2 .40 %,1.98%和 2 .43%。结论　本方法操作简便、重现性好、专属性强、准确可靠 ,可作为银杏萜内酯的定性定量分析方法。Object To develop a capillary GC-MS analytical method for identification and deter- mination of ginkgolide A, B, C and bilobalide (GA, GB, GC and BB) in Ginkgo biloba L. leaves. Methods The leave samples were extracted in ultrasonic bath with ethanol-water (20∶80). The extract was purified by liquid-liquid extraction with ethyl acetate followed by solid-phase extraction on a column mixed with acid Al 2O 3, active carbon and celite. The terpenes were trimethylsilylated by BSTFA (with 1% TMCS) for 60 min at 100 ℃ and determined by GC-MS with HP-5 MS capillary column in the selected-ion monitoring mode. The intense fragment ions were chosen as monitoring ions for quantitative analysis. Cholesterol was used as an internal standard. Column temperature gradient: initial temperature 180 ℃, maintained 1 min, and then increased at 20 ℃/min to 260 ℃, and finally at 2 ℃/min up to 300 ℃, maintained 2 min. Results The retention times of GA, GB, GC and BB were 13.7,14.3,15.3 and 6.8 min, the major fragmentation ions (monitoring) were at m/z 537, 625, 713 and 455 (299), the average recoveries of GA, GB, GC and BB were 102.0%, 99.4%, 96.0%, 96.3%, RSD were 0.54%, 2.40%, 1.98% and 2.43%, respectively. Conclusion This method is repeatable, specific, accurate and easy to operate. It is adoptable for quality and quantity analysis of terpene lactones from G. biloba leaves.

关 键 词：银杏叶 银杏萜内酯 银杏内酯 白果内酯 气相色谱-质谱 

分 类 号：R284.1[医药卫生—中药学]