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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 raw materials of Ginkgo biloba extract and to establish the determination method of terpene lactones in Wushenxitiao pills. Methods AB-8 macroporous resin was used to optimize the extraction of ginkgo leaf terpene lactones. The contents of four ginkgolides, ginkgolides, and ginkgolides were determined by HPLC-ELSD. The chromatographic conditions were optimized with a Diamonsil-C 18 column (250 mm × 4.6 mm, 5.0 μm) at a column temperature of 34 ° C. The mobile phase was eluted with methanol-0.2% formic acid at a flow rate of 0.7 mL · min ~ (-1); the detection of evaporative light scattering detector, the carrier gas pressure of 30 psi, the drift tube temperature of 80 ℃, at the same time determination Wushenxitiao pill in bilobalide, ginkgolides, ginkgolide A, Ginkgolide B content. Results Wushenxitiao dripping pills were pretreated with 60% ethanol extract of dry extract for the preparation of medicines. The four components (bilobalide and ginkgolide C, A, B) in drip pills were 4.77 ~ 47.70 mg · mL ~ (-1), 2.31-23.10 mg · mL -1, 4.79 ~ 47.94 mg · mL -1, 2.32 ~ 23.25 mg · mL -1, The area of the common logarithm (Y) showed a good linear relationship. The average recoveries of the four terpenoid lactones were 92.1%, 91.5%, 93.7% and 93.7%, respectively. The RSDs were 2.31%, 2.77%, 2.12% and 1.36%, respectively. Conclusion HPLC-ELSD determination of Wushen Xingnao dripping pill 4 kinds of terpene lactones separation of good specificity. This research can guarantee that the ingredients of Vitex Pinaneol can be controlled and the ingredients are controllable.