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参银复智制剂中银杏内酯的提取分离检测

         

摘要

Objective To seek the rapid and simple method for extracting, separating and detecting the effective component bilobalide and ginkgolide A, B and C from the monarch drug Ginkgo biloba leaves in Shenyinfuzhi Preparation. Methods The UPLC method was adopted for detecting the content. The chromatographic column was the Waters BEH C18 column ( 50 mm × 2. 1 mm, 1. 7 μm ) with the mobile phase of methanol-tetrahydrofuran-water ( 25:5:70 ) at a flow rate of 0. 3 mL/min. The column temperature was set at 30℃. The detection was carried out with the ELSD detector. The Ginkgo biloba leaves were extracted with 7 times 70%ethanol, refluxed twice, 3 h each time, the extract solution was combined, decompressed for recycling ethanol, adding 3 times the amount of water to pre-cipitate the impurity, and then filtrated by the macroporous adsorption resin D101, AB-8, D201 and polyamide resin respectively. The concentration and the use amount of the eluent were investigated. Results Polyamide resin was selected, after washing by 2 times of water, 10% ethanol elution with the 2-3 times of resin bed volume was performed. Then the eluent was collected, depressed, concentrat-ed and dried. The content was detected. The content of ginkgo terpene lactones was more than 35% and the yield rate of the effective parts was more than 90%. Conclusion This method is simple and rapid with high recovery rate, which provides a new method for ex-tracting, separating and detecting ginkgo terpene lactones from Ginkgo biloba leaves.%目的:寻找从参银复智制剂组方君药银杏叶中提取、分离、检测有效成分白果内酯和银杏内酯 A,B,C的快速简便的方法。方法采用超高效液相色谱法检测含量,色谱柱为Waters BEH C18柱(50 mm ×2.1 mm,1.7μm),流动相为甲醇-四氢呋喃-水(25:5:70),流速为0.3 mL/min,柱温为30℃,蒸发光散射检测器( ELSD )。银杏叶采用7倍70%乙醇回流提取2次,每次3 h,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酯D101,AB-8,D201及聚酰胺树脂,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倍树脂床体积的10%乙醇洗脱,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。结论该方法简便、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。

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