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

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

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=0.999 8)、0.04~0.4μg(r2=0.999 7)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。

Objective To establish the method for determination of emodin and physcion in sugar-free granules of Radix Polygoni Multiflori（zhishouwu）.Methods The high performance liquid chromatography（HPLC） analysis was performed on a Agilent 5TC-C18（150×4.6 mm,5 μm） 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 0.08-0.8 μ g（r_1=0.9998） and 0.04-0.4 μ g（r_2=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.