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目的:建立六合丹中大黄素的高效液相色谱法测定方法。方法:样品采用酸水解同时萃取的方法,加入盐酸加热回流,使苷类水解游离,再用氯仿进行萃取后,测定可由高效液相色谱-紫外可见检测器检测的游离型蒽醌成分总含量成分。使用DiamonsilC18色谱柱(150mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸溶液(85∶15),检测波长220nm,流速1.0mL.min-1,柱温25℃,进样量10μL。结果:大黄素在1.77~35.4mg.L-1范围内与峰面积积分值呈良好线性关系(r=0.999 9,n=5);平均加样回收率为100.71%,RSD为5.1%(n=6)。结论:本方法可靠、简便、灵敏、准确,适用于六合丹的质量控制。
Objective: To establish a method for the determination of emodin in Liuhe Dan by high performance liquid chromatography. Methods: The sample was extracted by acid hydrolysis simultaneously. Hydrochloric acid was heated to reflux and the glycosides were hydrolyzed and dissociated. After extracting with chloroform, the total content of free anthraquinones detected by high performance liquid chromatography - UV detector was determined. . A Diamonsil C18 column (150 mm × 4.6 mm, 5 μm) was used. The mobile phase was methanol-0.1% phosphoric acid solution (85:15). The detection wavelength was set at 220 nm and the flow rate was 1.0 mL.min-1. Results: Emodin showed a good linear relationship with the peak area integral value (r = 0.999 9, n = 5) in the range of 1.77-35.4 mg.L-1. The average recovery was 100.71% and the RSD was 5.1% (n = 6). Conclusion: The method is reliable, simple, sensitive and accurate and suitable for the quality control of Liuhe Dan.