乌参醒脑滴丸中银杏萜类内酯成分的质量控制研究  

Quality Control of Ginkgo Terpene Lactones in Wushen Xingnao Dropping Pill

作　　者：赵文静[1] 杨雄辉 范辉[1,2] 谭珍 邓德城 杨剑湖 贝伟剑[1] 

机构地区：[1]广东药学院中医药研究院,广东省代谢病中西医结合研究中心,广东广州510006 [2]广东药学院药科学院,广东广州510006 [3]国药集团冯了性(佛山)药业有限公司,广东佛山528000

出　　处：《中药新药与临床药理》2016年第1期113-118,共6页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：广东省重大科技专项项目;重大新药创制项目(2013A022100041);广东省教育部产学研结合项目(2012B091100193)

摘　　要：目的控制银杏叶提取物原料质量并建立乌参醒脑滴丸中萜类内酯成分的含量测定方法。方法采用AB-8大孔吸附树脂进行银杏叶萜类内酯提取优化,HPLC-ELSD法检测4种萜类内酯白果内酯及银杏内酯仁、A、B的含量,优选提取部位入药。优化色谱条件,采用Diamonsil-C_(18)(250 mm×4.6 mm,5.0μm)色谱柱,柱温34℃;以甲醇-0.2%甲酸水为流动相进行梯度洗脱,流速为0.7 mL·min^(-1);蒸发光散射检测器检测,载气压力为30 psi,漂移管温度为80℃,同时测定乌参醒脑滴丸中白果内酯、银杏内酯仁、银杏内酯A、银杏内酯B的含量。结果乌参醒脑滴丸优选60%乙醇提取部位干浸膏进行成药制剂,滴丸制剂中4种成分(白果内酯及银杏内酯C、A、B)分别在4.77~47.70mg·mL^(-1),2.31-23.10mg·mL^(-1),4.79~47.94mg·mL^(-1),2.32~23.25mg·mL^(-1)浓度的常用对数(X)与峰面积的常用对数(Y)呈良好的线性关系。其4种萜类内酯成分的平均回收率分别为92.1%,91.5%,93.7%,93.7%;RSD分别为2.31%,2.77%,2.12%,1.36%。结论 HPLC-ELSD法测定乌参醒脑滴丸4种萜类内酯分离度好,专属性强。该研究可保证乌参醒脑滴丸萜类内酯成分原料可控,成分可控。Objective To control the quality of Ginkgo biloba extract,and to establish a HPLC- evaporate lightscattering（ELSD） method for the determination of bilobalide,ginkgolide C,ginkgolide A and ginkgolide B in Wushen Xingnao dropping pill.Methods The macroporous resin AB- 8 was used to extract terpene lactones in Ginkgo biloba.The contents of four kinds of terpene lactones were monitored using HPLC-ELSD method.Chromatography was performed for the simultaneous determination of the four kinds of terpene lactones on a Diamonsil- C_（18）（250 mm×4.6mm,5.0 μm）column at 34 ℃.The mixture of 0.2%formic acid with methanol was used as the mobile phase,gradient elution was adopted,and flow rate was 0.7 mL·min^（-1）.An evaporate light-scattering（ELSD） was used as detector with drift tube temperature of 80 °C and gas pressure of 30 psi.Results The 60%ethanol dry extract of Wushen Xingnao dropping pill was used for assay.This HPLC- ELSD method was performed with good resolution and specificity.The results showed that the calibration curves of bilobalide,ginkgolide C,ginkgolide A,and ginkgolide B were linear in the range of 4.77~47.70 g·mL^（-1）,2.31-23.10 g·mL^（-1）,4.79-47.94 g·mL^（-1）,2.32-23.25 g·mL^（-1）.Their average recovery was 92.1%,91.5%,93.7%,93.7%,RSD was 2.31%（n=6）,2.77%（n=6）,2.12%（n=6）,1.36%（n=6）,respectively.Conclusion The HPLC- ELSD results for the four kinds of terpene lactones from60%ethanol dry extract of Wushen Xingnao dropping pill indicated that the terpene lactones of the pills are controlled,and components are guaranteed.

关 键 词：乌参醒脑滴丸 白果内酯 银杏内酯C 银杏内酯A 银杏内酯B HPLC-ELSD 大孔吸附树脂 

分 类 号：R284.1[医药卫生—中药学]