Abstract:

Objective　To establish a high performance liquid chromatography (HPLC) method to determine the content of emodin in modified Ganlu Xiaodu Dan. Methods　In this experiment, emodin in modified Ganlu Xiaodu Dan was extracted based on the protocol of Chinese Pharmacopoeia (2015 Edition). The HPLC separation was performed on the Agilent ZORMAX SB-C₁₈ chromatographic column (4.6 mm×150.0 mm, 5 μm); the injection volume was 10 μl; the gradient elution was conducted with methanol as mobile phase A and 0.1% phosphoric acid aqueous solution as mobile phase B for 15 minutes; the column temperature was room temperature; under the detection wavelength of 254 nm, the emodin content was detected. Results　The emodin in modified Ganlu Xiaodu Dan showed a good linear relationship with the peak area in the range of 2.000-8.000 μg (R²=0.999 8). The recovery rate was 100.17% (n=6); the relative standard deviation(RSD) was 1.87%; the average emodin content in modified Ganlu Xiaodu Dan was 13.936 8-14.831 1 µg/·g. Conclusions　The HPLC method can be used to determine the content of emodin in modified Ganlu Xiaodu Dan. The method is simple, rapid, accurate, and reliable, with ideal separation effect and good repeatability, and can provide experimental basis for the quality control of modified Ganlu Xiaodu Dan.

Key words:

High performance liquid chromatography, Modified Ganlu Xiaodu Dan, Content determination, Emodin

摘要：

目的　建立高效液相色谱（HPLC）法测定加味甘露消毒丹中大黄素的含量。方法　参考2015年版《中国药典》中的提取方法提取加味甘露消毒丹中的大黄素，采用Agilent ZORMAX SB-C₁₈色谱柱（4.6 mm×150.0 mm，5 μm），进样10 μl，以甲醇为流动相A，0.1%磷酸水溶液为流动相B，梯度洗脱15 min，柱温为常温，在254 nm的检测波长下测定大黄素含量。结果　加味甘露消毒丹中大黄素在2.000～8.000 μg（R²=0.999 8）范围内与峰面积呈良好线性关系，加样回收率为100.17%（n=6），相对标准差（RSD）为1.87%，该方中大黄素平均含量为13.936 8～14.831 1 µg/g。结论　建立的HPLC法可用于测定加味甘露消毒丹中大黄素的含量，该方法简便快捷、准确可靠，分离效果理想，重复性良好，为加味甘露消毒丹的质量控制提供实验依据。

关键词:

高效液相色谱法, 加味甘露消毒丹, 含量测定, 大黄素