文献类型：期刊文献

中文题名：消定膏质量标准提高研究

英文题名：Study on improving quality standard of Xiaoding Gao(消定膏)

作者：韩静[1];靳子明[2];窦霞[2];程芳[2];杨锡仓[2]

第一作者：韩静

机构：[1]甘肃中医药大学附属医院研究生部,甘肃兰州730020;[2]甘肃中医药大学附属医院制剂中心,甘肃兰州730020

第一机构：甘肃中医药大学第二附属医院

年份：2021

卷号：38

期号：4

起止页码：23

中文期刊名：甘肃中医药大学学报

外文期刊名：Journal of Gansu University of Chinese Medicine

基金：甘肃省中医药管理局科研课题(GZK-2015-17);甘肃中医药大学中青年科研基金项目(ZQ2017-3)。

语种：中文

中文关键词：消定膏;儿茶素;表儿茶素;芦荟大黄素;大黄酸;大黄素;大黄酚;大黄素甲醚;薄层色谱法;高效液相色谱法

外文关键词：Xiaoding Gao(消定膏);catechin;epicatechin;aloe-emodin;rhein;emo-din;chrysophanol;emodin methyl ether;thin layer chromatography(TLC);high performance liquid chromatography(HPLC)

摘要：目的提高消定膏的质量标准,有效控制制剂质量。方法采用薄层色谱(TLC)法对消定膏中大黄进行定性鉴别;采用高效液相色谱(HPLC)法对儿茶中儿茶素、表儿茶素,大黄中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚进行含量测定。以十八烷基硅烷键合硅胶(4.6 mm×250.0 mm,5μm)为填充剂,0.04 mol/L枸橼酸溶液-N,N-二甲基甲酰胺-四氢呋喃(45∶8∶2)为流动相测定儿茶中儿茶素和表儿茶素的含量;以甲醇-0.1%磷酸溶液(85∶15)为流动相测定大黄中芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量。结果TLC鉴别分离度高、专属性强、重现性好;儿茶素、表儿茶素的回归方程分别为Y=5.62987X+52.62137(r=0.9995),Y=6.52447X+4.95308(r=0.9995),线性范围分别为18.91~605.00,1.59~51.00μg,平均加样回收率分别为100.29%,98.74%,RSD分别为3.14%,3.04%;芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的平均加样回收率分别为95.36%,89.66%,93.22%,95.04%,91.41%,RSD分别为1.07%,2.17%,2.09%,2.48%,1.35%。结论本方法简单准确、专属性强,可为提高消定膏质量标准提供依据。
Objective To improve the quality standard of Xiaoding Gao(消定膏)and effectively control the quality of preparation.Methods Rhubarb in Xiaoding Gao was qualitatively determined by thin layer chromatography(TLC)method.The content determination of catechin and epicatechin in catechu and aloe-emodin,rhein,emodin,chrysophanol and emodin methyl ether in rhubard was carried out by high performance liquid chromatography(HPLC)method.The content determination of catechin and epicatechin in catechu was conducted using octadecylsilane bonded silica gel(4.6 mm×250.0 mm,and 5μm)as the stationary phase and a mixture of 0.04 mol/L citrate acid solution-N,N-dimethyl formamide and tetrahydrofuran(45∶8∶2)as the mobile phase.The content determination of aloe-emodin,rhein,emodin,chrysophanol and emodin methyl ether in rhubard was conducted by using a mixture of methanol and 0.1%phosphoric acid solution(85∶15)as the mobile phase.Results TLC identification had high resolution,strong specificity and good reproducibility.The regression equations of catechin and epicatechin were Y=5.62987 X+52.62137(r=0.9995)and Y=6.52447 X+4.95308(r=0.9995),respectively.The linear ranges were 18.91-605.00 and 1.59-51.00μg,respectively.The average recovery rate was 100.29%and 98.74%,respectively,with RSD of 3.14%and 3.04%,respectively.The average recovery rate of aloe-emodin,rhein,emodin,chrysophanol and emodin methyl ether was 95.36%,89.66%,93.22%,95.04%and 91.41%,respectively,with RSD of 1.07%,2.17%,2.09%,2.48%and 1.35%,respectively.Conclusion This method is simple,accurate and specific,whereby providing a basis for improving the quality standard of Xiaoding Gao.