HPLC-CAD法测定4种银杏叶制剂中萜类内酯类成分的含量

Determination of ginkgolides in four kinds of Ginkgo leaf preparations by HPLC-CAD

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(150mm×4.6 mm,2.7μm)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、1.013μg·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,2.7μm)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 1.545μg·m L(-1),2.169μg·m L-1,0.931μg·m L-1,and 1.013μg·m L-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.