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目的:完善一清片的质量控制方法。方法:采用薄层色谱法对处方黄芩、大黄进行定性鉴别;采用高效液相色谱法测定黄芩苷、大黄素、大黄酚的含量;建立一清片中表小檗碱、黄连碱、巴马汀和小檗碱的一测多评方法;同时采用外标法测定上述4种生物碱的含量,比较计算值与实测值之间的差别。结果:薄层色谱中可检出黄芩、大黄,专属性强,阴性无干扰;本方法大黄素、大黄酚线性范围分别为5.21~156.24,10.96~328.80 ng;平均回收率分别为94.49%,93.88%;RSD分别为1.2%,1.6%(n=6);可用一测多评法测定一清片中4种原小檗碱型生物碱的含量,2种测定方法差异无显著。结论:本试验的方法可靠,结果准确,可运用于一清片的质量控制。
Objective: To improve a quality control methods. Methods: The prescriptions of Scutellaria baicalensis and Rheum officinale were identified by TLC. The contents of baicalin, emodin and chrysophanol were determined by HPLC. The contents of berberine, berberine, palmatine And berberine a test evaluation method; at the same time using the external standard method for the determination of the above four kinds of alkaloids, the calculated value and the difference between the measured value. Results: Scutellaria baicalensis and Rhubarb could be detected in thin layer chromatography with strong specificity and no negative interference. The linear ranges of emodin and chrysophanol in this method were 5.21 ~ 156.24 and 10.96 ~ 328.80 ng, respectively. The average recoveries were 94.49% and 93.88%, respectively %; RSD were 1.2%, 1.6% (n = 6); Determination of four kinds of protoberberine alkaloids in a clear film can be more than one evaluation method, two kinds of determination method was no significant difference. Conclusion: The method of this test is reliable and accurate. It can be applied to the quality control of a clear piece.