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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 establish an UPLC method for the simultaneous determination of 3 C21 steroidal ester glycosides (F, G, Methods: The samples were extracted by methanol and analyzed by UPLC-PDA. The samples were eluted with ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) using a Waters Acquity UPLC system. The mobile phase consisted of acetonitrile-water with gradient elution , Flow rate of 0.4 mL.min-1, detection wavelength of 220 nm, column temperature 30 ℃, injection volume 2μL. Results: Three C21 steroidal ester glycosides of F, G and H in the Radix Bupleuri showed a good linearity (r ≥ 0.995) within the detection range. The average recoveries (n = 3) ranged from 98.2% to 104.1% Between, RSD is not more than 1.1%. Conclusion: UPLC separation and reproducibility is good, fast and simple, and can be used as a reference method for the quality control of Geosan.