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目的:研究微米大黄炭定性、定量检测方法,建立微米大黄炭的质量控制方法。方法:用HPLC法测定微米大黄炭中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚含量。采用Fortis universil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇(A)-0.2%磷酸溶液(B)进行梯度洗脱,检测波长254 nm,流速1 ml·min-1。结果:芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚分别在0.084 8~0.848,0.089 6~0.896,0.089 6~0.896,0.124 4~1.244,0.091 4~0.914μg·ml-1范围内线性关系良好。平均回收率(n=6)分别为98.83%,99.54%,98.99%,99.17%,100.27%;RSD分别为1.05%,0.61%,1.61%,1.83%,1.38%。结论:本方法分析简便、准确,重现性好,可作为该制剂的质量控制。
Objective: To study the method of qualitative and quantitative detection of micron rhubarb carbon and establish the quality control method of micron rhubarb carbon. Methods: The contents of aloe-emodin, rhein, emodin, chrysophanol and physcion in micron rhubarb charcoals were determined by HPLC. The mobile phase consisted of a gradient of methanol (A) - 0.2% phosphoric acid (B) with a Fortis universil C18 (250 mm × 4.6 mm, 5 μm) column at a detection wavelength of 254 nm and a flow rate of 1 ml · min -1. Results: Aloe-emodin, rhein, emodin, chrysophanol and physcion were detected in the range of 0.084 8 ~ 0.848,0.089 6 ~ 0.896,0.089 6 ~ 0.896,0.124 4 ~ 1.244,0.091 4 ~ 0.914μg · ml -1 Linear relationship within the range of good. The average recoveries (n = 6) were 98.83%, 99.54%, 98.99%, 99.17% and 100.27%, respectively. The RSDs were 1.05%, 0.61%, 1.61%, 1.83% and 1.38%, respectively. Conclusion: The method is simple, accurate and reproducible, which can be used as the quality control of the preparation.