双波长-UPLC法同时测定胡黄连中4个环烯醚萜类成分的含量

Simultaneous determination of four iridoid ingredients in Picrorhizae Rhizoma by dual-wavelength UPLC

目的:建立同时测定中药材胡黄连中环烯醚萜类成分胡黄连苷Ⅰ、Ⅱ、Ⅲ和Ⅳ含量的双波长-UPLC法。方法:采用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),柱温:28℃;流动相:乙腈-0.5%乙酸水溶液,梯度洗脱;流速:0.4 mL·min^-1;检测波长分别为275 nm(胡黄连苷Ⅰ和Ⅱ)、295 nm(胡黄连苷Ⅲ和Ⅳ)。结果:胡黄连苷Ⅰ、Ⅱ、Ⅲ和Ⅳ在质量浓度为4.44~88.72μg·mL^-1(r=1.000)、17.23~344.61μg·mL^-1(r=1.000)、1.97~39.35μg·mL^-1(r=1.000)、1.98~39.51μg·mL^-1(r=1.000)范围内与峰面积线性相关,平均回收率分别为102.4%、98.8%、96.5%、101.9%,RSD分别为1.0%、2.3%、1.1%、2.0%。结论:该方法操作简便、快速、重复性好、结果准确可靠,适用于胡黄连的质量控制。

Objective:To establish a dual-wavelength UPLC method for simultaneous determination of iridoids including picroside Ⅰ,picroside Ⅱ,picroside Ⅲ and picroside Ⅳ in Chinese herbal medicine Picrorhizae Rhizoma. Methods:The separation was performed on a Waters ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm)and the column temperature was set at 28℃. The mobile phase was composed of acetonitrile and 0.5% acetic acid with gradient elution at a flow rate of 0.4 mL·min^-1. The detection wavelength was set at 275 nm for picroside Ⅰ and picroside Ⅱ and at 295 nm for picroside Ⅲ and picroside Ⅳ. Results:The calibration curves were linear within the range of 4.44-88.72 μg·mL^-1(r=1.000)for picroside Ⅰ,17.23-344.61 μg·mL^-1(r=1.000)for Picroside Ⅱ,1.97-39.35 μg·mL^-1(r=1.000)for picroside Ⅲ,1.98-39.51 μg·mL^-1(r=1.000)for picroside Ⅳ. The average recovery rates of picroside Ⅰ,picroside Ⅱ,picroside Ⅲ and picroside Ⅳ were 102.4%,98.8%,96.5% and 101.9% with RSD values of 1.0%,2.3%,1.1% and 2.0%,respectively. Conclusion:The method is simple,rapid,reproducible,accurate and reliable,and can be used for quality control of Picrorhizae Rhizoma.