洁康舒洗剂的质量标准研究

Study on Quality Standard of JKS Lotion

目的 制订洁康舒洗剂的质量标准。方法 采用薄层色谱法 (TLC)对该制剂中大黄、黄柏、徐长卿、冰片等主药进行定性鉴别 ,其中大黄的薄层鉴别以石油醚 -乙酸乙酯 -甲酸 (10∶3∶1)为展开剂 ;黄柏以正丁醇 -冰醋酸 -水 (10∶1∶1)为展开剂 ;徐长卿以环乙烷 -醋酸乙酯 (4∶2 )为展开剂 ;冰片以石油醚 -乙酸乙酯 (6∶2 )为展开剂。用高效液相色谱法测定该制剂中大黄酸、大黄素及大黄酚的含量 ,色谱柱为SymmetryC18柱 (3.9mm× 15 0mm ;5 μm) ,SymmetryC18预柱 (3.9mm× 2 0mm)流动相为甲醇 -水 -磷酸 (82∶18∶0 .1) ,柱温 2 4℃ ,检测波长 4 32nm ,流速为 1.0ml/min。结果 洁康舒洗剂中的有效成分与相应对照品均呈相同的鉴别反应 ,大黄酸、大黄素及大黄酚的浓度分别在 7.6 0～ 38.0 0 μg·ml-1(r =0 .9994 ) ;1.75～ 8.75 μg·ml-1(r =0 .9999) ;2 .4 0～ 12 .0 0 μg·ml-1(r =0 .9999)范围内线性关系良好。平均回收率大黄酸为 98.0 2 % ,RSD =1.78% ;大黄素为 96 .6 3% ,RSD =1.2 0 % ;大黄酚为 97.0 5 % ,RSD =1.15 % (n =5 )。结论 该制剂定性反应灵敏、TLC鉴别专属性强、定量结果准确、重现性好。本实验方法为洁康舒洗剂质量标准的制订提供了科学依据。

Aim To study the quality standard of JKS lotion.Methods The Dahuang,rhubarb,Huangbai,XuChangQing,Boinpian in JKS lotion were identified by TLC.The reference substances of rhubarb were Rhen,Emodin,Chrysophanol.Developer were petroleum ether,ethyl acetate,formic acids(10∶3∶1).The reference substance of Cortex phellodendri was berberine hydrochloride.Developer were n-butyl alcohol-acetic acid-water(10∶1∶1).The reference substance of radix cynanchi paniculati was paeonol.Developer was cyclohexane and ethyl acetate(4∶2).The borneol selects the crude drugs of contrast for use.Developer were petrolenm ether and ethyl acetate(6∶2),HPLC was adopted to determine the contents of Rhen,Emodin,Chrysophanol in JKS lotion.With chromatographic column for Symmetry C 18 column(3.9×150mm,5μm).Symmetry C 18 in advance column(3.9×20mm),flow phase:methanol-water-phosphoric acid(82∶18∶0.1).The temperature of Column was 24℃.Detection wavelength was 432nm.The speed of flow was 1.0ml/min.Results JKS lotion and corresponding contrast product present the same distinguishes and reacts.The density of Rhen,Emodin,Chrysophanol in JKS lotions difference in 7.60～38.00μg·ml -1 (r=0.999 4),1.75～8.75μg·ml -1 (r=0.999 9),2.4～12.00μg·ml -1 (r=0.999 9).The linear relationship is good.Their average recovery rate in JKS lotions:Rhen was 98.02%,RSD=1.78%.Emodin was 96.63%,RSD=1.20%;chrysophanol was 97.05%,RSD=1.15%,(n=5).Conclusions The method is sensitivly and selective.The quantitative date are reliable.This method offers the intact experiment basis of JKS lotion quality standard.