银杏雄株叶片萜内酯类化合物的HPLC检测分析

Test and Analysis on Ginkgolides and Bilobalid in the Leaves of Male Plants in Ginkgo by HPLC

目的:银杏叶萜内酯类化合物具重要的药用与保健开发利用价值。方法:在银杏最佳采叶期随机采取银杏叶片,经超声波70%乙醇水溶液提取、石油醚与正己烷萃取,再经ADS-17大孔树脂柱与酸性氧化铝柱纯化,以水∶甲醇∶四氢呋喃=7∶2∶1(V/V)为流动相,采用Waters ODS C18柱(250mm×416mm,5μm)进行HPLC分析:0.6ml/min流速、219nm检测波长、26℃检测温度、15μl进样量。结果:GA、GB、GC和BB分别在23～460μg/ml、21～420μg/ml、22～440μg/ml和27～540μg/ml范围内呈线性相关,最小检出量0.5μg,回收率90.74%～102.38%,RSD 1.63%～4.2%。GBE3得率1%,GA、GB、GC、BB占GBE3的12.55%,超过GBE761的6%国际标准。结论:该HPLC检测分析技术与方法适用于银杏叶片萜内酯类化合物的提取、纯化和检测。

Objective：Ginkgolides and bilobalid in the leaves of male Ginkgo boliba L.has important medicinal value and health care utilization.Method：The crude GBE produced from extraction of the leaves of the male Ginkgo boliba L.,which were collected in the best of leaf collecting time with 70% alcohol solution by ultrasonic method was used to be extracted with petroleum ether and n-Hexane,then purified with ADS-17 and Aluminum oxide for HPLC analysis with a mobile phase consisting of water∶methanol∶THF=7∶2∶1（V/V）.The HPLC assay was conducted with waters ODS C18 column at a flow rate of 0.6 ml/min and UV detection at 219 nm,the test temperature of 26℃ and the injection volume of 15μl.Result：The linearity range for GA,GB,GC,BB were obtained from 23 to 460μg/ml,21 to 420μg/ml,22 to 440μg/ml,27 to 540μg/ml respectively.The limit of detection for them was 0.5μg.The recovery rates of them were from 90.74% to 102.38 %.The RSD were from 1.63% to 4.2%.The GBE3 yield of the leaf samples was 1% and the total of GA,GB,GC,BB account 12.55% GBE3 which had exceeded the international standard of 6% in GBE761.Conclusion：The above HPLC method of test and analysis is applicable for the extraction,purification and detection of Ginkgolides and bilobalid in the leaves of Ginkgo.