清火片标准中检测方法的提高与修订研究

Improvement and revision of the test methods in the specification of Qinghuo Tablets

目的:提高清火片的质量标准。方法:采用薄层色谱法,以靛玉红、大黄对照药材和大黄酸、薄荷脑及土大黄苷作为指标进行相关药味的定性鉴别及伪品大黄的检查;采用高效液相色谱法,以大黄素和大黄酚为指标成分进行大黄中总蒽醌和结合蒽醌的定量检测。结果:薄层色谱方法斑点清晰,分离度良好;大黄素和大黄酚分别在1.674～41.849μg·mL^(-1)、2.594～64.860μg·mL^(-1)浓度范围内呈良好的线性关系;游离大黄素、游离大黄酚、总大黄素和总大黄酚的平均加样回收率(n=6)分别为101.55%、102.59%、102.13%、101.91%。总蒽醌含量为0.383～1.115 mg·片^(-1),结合蒽醌含量为0.063～0.514 mg·片^(-1)。结论:本实验所建立的定性定量方法快速准确、重现性良好,为完善清火片的质量标准提供了依据。

Objective:To improve the specification of Qinghuo Tablets.Methods:Indirubin,radix rheum,rhein and rhaponiticin as index components were qualitatively identified by TLC.Counterfeit radix rheum was inspected by TLC as well.Totalanthraquinone and combined anthraquinone in Radix Rheumwere determined by HPLC with emo- din and chrysophanol as index components.Results:All TLC spots were clear and separated well.The linear ranges of emodin and chrysophanolfell intol.674 -41.849 and 2.594 -64.860 μg·mL^-1,respectively.The average recoveries (n =6 )of free emodin,free chrysophanol,total emodin and total chrysophanolwere 101.55%, 102.59%,102.13%and 101.91%,respectively.The contents of total anthraquinone and combined anthraquinone were 0.383 -1.115 mg per tabletand 0.063 -0.514 mg per tablet,respectively.Conclusion:The established qualitative and quantitative methods were rapid,accurate and reproducible.It can provide basis for specification improvement of Qinghuo Tablets.