超声提取法测定熊胆消炎胶囊中大黄素和大黄酚的含量

Quantitative analysis of emodin and chrysophanol in Xiongdan Xiaoyan capsule by Ultrasonic extraction

目的 建立熊胆消炎胶囊中大黄素和大黄酚的含量测定方法。方法 采用超声提取RP -HPLC法测定 ,用Shim packCLC -ODS柱 (6 0mm× 15 0mm ,5 μm) ,以甲醇 - 0 1%磷酸溶液 (85∶15 )为流动相 ,检测波长 2 5 4nm。 结果 大黄素的线性范围为 4 0 88～ 81.76ng(r=0 .9999) ,平均回收率为 99 3% ,RSD =0 93% (n =9) ;大黄酚的线性范围为 8 2 72～ 16 5 4 4ng(r =0 9999) ,平均回收率为 99 5 % ,RSD =1 86 % (n =9)。测定大黄素方法精密度RSD =0 .6 0 % (n =5 ) ,测定大黄酚RSD =0 6 5 %(n =5 )。结论 所用方法测定样品的分离效果佳 ,灵敏度高 ,重复性好 ,结果准确可靠。

OBJECTIVE To establish a quantitative method for emodin and chrysophanol in Xiongdan Xiaoyan capsules by RP-HPLC.METHODS The samples were extracted by ultrasound wave and separated by Shim-pack CLC-ODS column(6.0 mm×150 mm,5 μm)with methanol-0.1% phosphoric acid (85∶15)as mobile phase and detected at UV 254 nm.RESULTS The calibration curve of emodin was linear in the range of 4.088-81.76 ng(r=0.9999);The average recovery of sample was 99.3% with RSD of 0.93%(n=9);The calibration curve of chrysophanol was linear in the range of 8.272-165.44 ng(r=0.9999).The average recovery of sample was 99.5%,with RSD of 1.86%(n=9).Precisions of the analytical method were 0.60%(n=5)for emodin and 0.65%(n=5)for chrysophanol,respectively.CONCLUSION The method is good in the aspect of separable efficiency,reproducibility and sensitivity.