目的:建立同时测定民族药材隔山消中3个C21甾体酯苷(白首乌新苷F、G和H)的UPLC分析法。方法:样品经甲醇超声提取后,用UPLC-PDA进行分析检测;采用Waters Acquity UPLC系统,ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,流动相为乙腈-水,梯度洗脱,流速为0.4 mL.min-1,检测波长220 nm,柱温30℃,进样量2μL。结果:白首乌新苷F、G和H 3个C21甾体酯苷在检测范围内均呈良好线性(r≥0.9995);平均加样回收率(n=3)在98.2%~104.1%之间,RSD均不大于1.1%。结论:UPLC分离效果及重复性好,且快速、简便,可作为隔山消药材质量控制的参考方法。
Objective: To develop an ultra performance liquid chromatography (UPLC) method to simultaneously determine three pregnane glycosides( cynanauriculosides F, G, H) in Cynanchum auriculatum. Methods: After the untrasonie -assisted extraction with methanol, the analyses were performed on a Waters UPLC system, equipped with a binary solvent manager, a sampler manager, a column compartment and a PDA detector. An ACQUITY UPLC BEH Cls column(2.1 mm ~100 ram, 1.7 pin) was used for all analyses. The investigated compounds were separa- ted with the mobile phases of water and acetonitrile in gradient elution, with a flow rate of 0.4 mL ~ min-l. The temperature of column was set at 30 ~C, and the injection volume was 2 p~L. The detection wavelength was set at 220 nm. Results: The investigated compounds including cynanauriculoside F, G and H had good linearity( ≥0. 9995) over the tested ranges. The average recoveries( n = 3) were 98.2% to 104.1% with RSDs ≤1.1%. Conclusion: The developed UPLC method is simple, sensitive and accurate with good repeatability, which is available for quality control of raw material of Cynanchum auriculatum.