HPLC-CAD法测定4种银杏叶制剂中萜类内酯类成分的含量

目的：建立高效液相-电雾式检测器（HPLC-CAD）检测4种银杏叶制剂（银杏叶片、银杏叶分散片、银杏叶胶囊和银杏叶滴丸）中萜类内酯类成分的含量。方法：采用Poroshell 120 SB-C₁₈色谱柱（150 mm×4.6 mm，2.7 μm）分离，以甲醇-水为流动相进行梯度洗脱，柱温35℃，CAD检测器雾化温度为35℃，载气N₂，压力438.5 kPa。结果：该方法对白果内酯、银杏内酯A、银杏内酯B、银杏内酯C 4个萜类内酯类成分的检测下限分别为1.545、2.169、0.931、1.013 μg·mL–1；线性良好，相关系数均大于0.999；精密度、稳定性和重复性RSD均小于2.0%；4个萜类内酯成分在各品种制剂中加样回收率分别为103.4%~105.3%、95.8%~104.0%、96.1%~102.0%、97.6%~101.5%。结论：本实验建立的方法重复性良好，准确度高，操作简单，灵敏度高，可用于银杏叶制剂中萜类内酯类成分的含量测定。

Objective:To establish an HPLC-CAD method for determination the content of ginkgolides in four kinds of ginkgo leaf preparations(Ginkgo leaf tablets,Ginkgo leaf dispersible tablets,Ginkgo leaf capsules,Ginkgo leaf Dripping pills).Methods:The chromatographic process was performed on a Poroshell 120 SB-C₁₈ column(150 mm×4.6 mm,2.7 μm)with the mobile phase of methanol-water with gradient elution.The column temperature was 35℃.The detector was CAD(the spray temperature was 35℃),at gas pressure of 438.5 kPa;The methodology validation was made and determination was carried out with 18 batches of samples of four different preparations of Ginkgo leaf preparations.Results:The LODs of four ginkgolides,including bilobide,ginkgolide A,ginkgolide B,and ginkgolide C were 1.545 μg·mL^-1,2.169 μg·mL^-1,0.931 μg·mL^-1,and 1.013 μg·mL^-1, respectively.The linearity was good and the correlation coefficients were all above 0.999;RSDs of precision,stability and repeatability were less than 2.0%;the average recoveries of four ginkgolides were 103.4%-105.3%,95.8%-104.0%,96.1%-102.0%,and 97.6%-101.5% respectively.Conclusion:The method has good reproducibility,high accuracy,simple operation and high sensitivity.It can be used for the determination of ginkgolides in Ginkgo leaf preparations.

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