动态超声辅助萃取与HPLC联用测定淫羊藿中黄酮类化合物

建立了动态超声辅助萃取与高效液相色谱在线联用系统,用于测量淫羊藿中黄酮类化合物。萃取过程在一个循环体系中完成,萃取完成后,通过采样环采集20μL萃取液,萃取液被流动相载入色谱系统进行分离检测。4种黄酮类化合物用HPLC–MS区分,通过比较色谱峰面积选择优化萃取条件。选择50℃的水浴温度,50%的乙醇作为萃取剂,萃取剂流速为1.5 mL/min,萃取时间为8 min,样品量为15 mg。用该法测量淫羊藿样品中4种黄酮类化合物,日内、日间精密度分别为1.05%～2.05%,0.30%～3.63%(n=6)。淫羊藿中的主要化合物淫羊藿苷的加标回收率为95.2%。该方法可用于测量淫羊藿中的黄酮类化合物。

Determination of Flavonoids in Epimedium Koreamum Nakai by Dynamic Ultrasonic-assisted Extraction System Coupled with HPLC

The dynamic ultrasonic-assisted extraction （DUAE） system coupled with HPLC was used for determination of four flavonoids in epimedium koreamum nakai. The extraction was performed in a recirculating system. When the extraction was completed, the extract （20 μL） was driven to the analytical column by mobile phase and measured by a UV detector. The four flavonoids were identified by HPLC-MS. The extraction parameters of the procedure were optimized by comparison with the peak areas of HPLC. The extraction temperature was 50℃in water bath, the extract solvent was 50%ethanol, the extractant flow rate was 1.5 mL/min, the extraction time was 8 min, and the quantity of the sample was 15 mg. Four flavonoids were measured by the method, the RSD of intra-day and inter-day were 1.05%-2.05%and 0.30%-3.63%（n=6）, respectively. The method was applied to determine icariin which was major component in the herb, and the added recovery was 95.2%. The method was successfully applied to the determination of flavonoids in epimedium koreamum nakai.