HPLC法同时测定制首乌无糖颗粒中大黄素、大黄素甲醚的含量

目的：建立制首乌无糖颗粒中大黄素、大黄素甲醚的含量测定方法。方法采用Agilent 5TC-C18(150×4.6 mm，5μm)色谱柱，流动相为甲醇-0.1%磷酸(80：20)，流速1.0 mL/min，检测波长254 nm，柱温25℃。结果大黄素和大黄素甲醚分别在0.08~0.8μg (r1=0.9998)、0.04~0.4μg (r2=0.9997)范围内与峰面积呈良好的线性关系，平均加样回收率分别为100.04%、99.58%，RSD分别为0.77%，0.71%。3批样品中大黄素的含量分别为0.159 mg/g、0.161 mg/g、0.170 mg/g，大黄素甲醚的含量分别为0.055 mg/g、0.064 mg/g、0.072 mg/g。结论本方法准确、专属性好、重复性好，可作为制首乌无糖颗粒质量控制方法之一。

Simultaneous determination of emodin and physcion in sugar-free granules of Radix Polygoni Multiflori (Heshouwu) by HPLC

Objective To establish the method for determination of emodin and physcion in sugar-free gran-ules of Radix Polygoni Multiflori (zhishouwu). Methods The high performance liquid chromatography (HPLC) analy-sis was performed on a Agilent 5TC-C18 (150×4.6 mm, 5μm) with methanol-0.1%phosphoric acd solution (80:20) as the mobile phase:flow rate:1.0 mL/min;column temperature:25℃;detection wavelength:UV 254 nm. Results The emodin and physcion respectively showed the good linear relationship with peak area within the range of 0.08-0.8μg (r1=0.9998) and 0.04-0.4 μg (r2=0.9997). The average recoveries of samples were 100.04% and 99.58%, respectively, with the relative standard deviation (RSD) of 0.77% and 0.71%, respectively. The content of emodin in three samples were 0.159 mg/g, 0.161 mg/g and 0.170 mg/g, and the content of physcion in three samples were 0.055 mg/g, 0.064 mg/g and 0.072 mg/g. Conclusion The method is accurate, with good specificity and good reproducibility, and can be used as one of the quality control methods for the sugar-free granules of Radix Polygoni Multiflori.