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出 处:《实用医药杂志》2014年第4期336-339,共4页Practical Journal of Medicine & Pharmacy
基 金:苏州卫生职业技术学院课题(szwzy201119);江苏省优秀骨干教师境外研修成果之一
摘 要:目的 银杏叶是参银复智制剂的君药,寻找快速简便的方法从银杏叶中提取分离检测有效成分白 果内酯和银杏内酯A、B、C.方法 采用超高效液相色谱法(UPLC),色谱柱:waters BEH C18,2.1×50 mm,1.7 μm;流动相:甲醇-四氢呋喃-水(25∶5∶70);流速0.3 ml/min;柱温:30℃;蒸发光散射检测器(ELSD).银杏叶采用7倍70%乙醇溶液回流提取2次,3h/次,合并提取液,减压回收乙醇,加3倍量水使沉淀,过滤,滤液分别上大孔吸附树脂D101、AB-8、D201、聚酰胺树脂,考察洗脱剂的浓度和用量.结果 选择聚酰胺树脂,2倍水洗后,用2~3倍树脂床体积10%乙醇溶液洗脱,收集洗脱液,减压浓缩干燥,检测含量,银杏萜类内酯的含量都在35%以上,有效部位得率在90%以上.结论 超高效液相色谱法简便快速、回收率高,为银杏叶中内酯类物质的提取分离检测提供了一种新方法.Objective To establish a simple and rapid method for extraction,separation and detection bilobalide and ginkgolide A,B,and C from Ginkgo biloba leaves. Methods Ultra performance liquid chromatograph with evaporative light scanning detector (UPLC-ELSD) method was adopted:waters BEH C18 (2.1×50 mm,1.7 μm) column,mobile phase: methanol-tetrahydrofuran-water (25:5:70) at a flow rate of 0.3 ml/min, column temperature 30 ℃. The detection was carried out with ELSD detector. The Ginkgo biloba leaves was extracted with 7 times of 70% ethanol,refluxed for 2 hours each time,the extraction solution was combined,removed the ethanol under vacuum,added 3 times of water to precipitate the impurity,the filtrate was through the DIO1 resin column,AB-8 resin column,D201 resin column and polyamide column respectively. Results The optimized conditions to prepare Yinxing terpenelactones in the Ginkgo biloba leaves filtrate was through polyamide column,washed with 2 times water and then eluted with 2-3BV of 10% ethanol,the collected elution of water and ethanol were concentrated under vacuum,then the Yinxing terpenelactones were obtained,with the concentration at more than 35% and the yield rate at more than 90%. Conclusion Above method which is simple and rapid can provide a new way to extract,separate and detect Yinxing terpenelaetones from Ginkgo biloba leaves.
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