Study On Preparation Process And Quality Control Of Qingre Xiehuo Mixture

Objective:The prescription of Qingre Xiehuo mixture is derived from the folk prescription Sanjiao Xiehuo decoction,which consists of scutellariae redix,sophora alopecuroides redix,rhei franzenbachii redix et rhizoma,glycyrrhizae radix et rhizoma,gypsum fibrosum and talct pulvis.This prescription has the functions of clearing heat,relieving cough and eliminating phlegm,and benefiting the pharynx.It can clear internal heat,remove moisture and detoxification,which is clinically used to treat internal heat,cough,phlegm and asthma,sore throat,dry stool,etc.The purpose of this project is to explore the extraction and preparation processes of the Qingre Xiehuo mixture,and to conduct quality control and stability studies to provide a reference for future large-scale production.Methods:With reference to the relevant provisions of the 2015 edition of the Chinese Pharmacopoeia and Chinese Veterinary Pharmacopoeia,in the study of the water extraction process,the orthogonal test method was used to investigate the three factors of water addition,decoction times and decoction time.The optimal extraction process of the mixture was obtained and verified by data analysis.The gradient method was used to investigate the concentration volume,p H value and the amount of solubilizer in the molding process.The preparation process was determined by optimizing the molding conditions.In the study of quality control methods,a thin-layer chromatography identification method based on the relevant indexes of the four medicinal materials of scutellaria baicalensis,the root of sophora alopecuroides,rheum franzenbachii munt and liquorice was established.Through the system adaptability test,linear relationship test,precision test,repeatability test,solution stability test,sample recovery test,durability test,etc.,the HPLC method for determining baicalin in Qingre Xiehuo mixture was determined.Stability studies such as influencing factor tests,accelerated tests,and long-term tests have been performed.Results:The preparation process of the Qingre Xiehuo mixture was as follows:add 8 times the amount of water and extract 3 times for 1.5h each time,pass the 200 mesh sieve,combine the filtrates,concentrate under reduced pressure to 700m L,add 0.2%potassium sorbate,adjust the p H range to 4.5～5.5,add14m L of 10-fold diluted tween-80 solution,heat to reflux for 30 min,cool and precipitate for 72 hours,and aliquot into 100m L bottles.In the study of quality standards,thin layer chromatography of scutellaria baicalensis,the root of sophora alopecuroides,rheum franzenbachii munt and liquorice was identified as qualitative identification methods.The content of baicalin in the mixture was determined by high performance liquid chromatography.The linear regression equation of baicalin in the range of 0.12～0.96μg was:Y=51.4728X-0.3712,r=1.000,and the sample recovery was 98.22%.The established content determination method is reasonable and feasible.The RSD of three batches of pilot sample content was within 2%.The content of baicalin in Qingre Xiehuo mixture should not be less than 1.4175mg·m L^-1.The test results of influencing factors indicate that the Qingre Xiehuo mixture is stable under high temperature,high humidity and strong light conditions.Accelerated tests and long-term tests have shown that the mixture has good stability,and the validity period can be tentatively set to 12 months.Conclusion:The preparation process of the Qingre Xiehuo mixture is determined.The process is reasonable,feasible,easy to operate,and low in cost.A preliminary quality standard was developed.The baicalin content was determined by high performance liquid chromatography.The method is highly sensitive,accurate and repeatable.A thin-layer identification method for scutellaria baicalensis,the root of sophora alopecuroides,rheum franzenbachii munt and liquorice was identified.The method has the characteristics of strong specificity and easy operation.The stability investigation shows that the stability of the finished product is good,which provides a basis for controlling its product quality.