Study On The Preparation Technology And Quality Control Method Of Biminting Granule

ObjectivesAllergic rhinitis(AR)is a type of inflammation in the nose which occurs when the immune system overreacts to allergens in the air.Signs and symptoms include a runny or stuffy nose,sneezing,red,itchy,and watery eyes,and swelling around the eyes.In those years,PM 2.5,the hottest topic in the society,is a factor that can not be ignored to cause the AR.The original prescription of BIMINTING Granule is a clinical prescription,which is composed of Saposhnikoviae Radix,Magnoliae Flos,Forsythiae Fructus,Lonicerae Flos and Glycyrrhizae Radix.The prescription has effect on the treatment of Allergic rhinitis in clinic.This study is focused on optimizing the preparation process and uniforming preliminary quality standard research in the modern pharmaceutical method.MethodsThere are mainly three parts in this study,which are Extraction and Concentration process,granulation process and quality standard of BIMINTING Granule.1.Extraction and Concentration:Due to physical and chemical properties of herbal medicines.At first,optimize the process of extraction of mixed volatile oil from Saposhnikoviae Radix,Magnoliae Flos and Forsythiae Fructus by single factor experiments.And then,volatile oil inclusion of β-cyclodextrin by orthogonal design was adopted to examine effects of charge ratio of volatile oil and β-CD,inclusion temperature and inclusion time on the inclusion process.Secondly,combining the crude with other two herbs,which are Lonicerae Flos and Glycyrrhizae Radix in water to extract in orthogonal test optimization to explore how solvent times,extraction duration and extraction times affect the water extraction,further determine the optimum conditions for extraction.According to transfer rate of phillyrin and chlorogenic acid,the alcohol precipitation process was optimized by single factor experiments.2.Granulation:The wet granulation was used in this study.According to the molding rate and moisture absorption,the granulation was optimized by the orthogonal experiment method in impact of types of supplementary material,medicine auxiliary ratio and ethanol concentration.3.Quality standard research:This study identified all herbs by TLC method.And also,the study determined the content of phillyrin and chlorogenic acid by HPLC method.Combined those two results,the quality standards were established.Results1.Result of Extraction and Concentration:The process of extraction of mixed volatile oil conditions were soaking fine powder extracted 5 hours with 10 folds the amount of water.The process of inclusion of mixed volatile oil conditions were as follows:Mixed volatile oil-β-cyclodextrin ratio was 1:10;inclusion temperature was 50℃;inclusion time was 2 hours.Extraction process:Adding 8 times water,1 hour heating reflux for 2 times.Alcohol-precipitation process:The filtrate was concentrated to a relative density of 1.05-1.10(60℃),the alcohol concentration of 60%and Placed for 24hours.2.Result of Granulation:wet granulation,dextrin as excipient,drugs and excipient ratio was 1:1.5,85%ethanol and environmental critical relative humidity at 70%or less.3.Quality control method established:This study determined the TLC qualitative identification method of five herbs.The high performance liquid content determination method for phillyrin were as follow:Kromasil C18(250×4.6mm,5μm)chromatographic column;mobile phase was acetonitrile-water(22:78);column temperature was 35℃;the flow rate of 1.0ml/min;detection wave length of 277nm.The average content of phillyrin in BIMINTING Granule is 0.52mg/g.The high performance liquid content determination method for chlorogenic acid were as follow:Kromasil C18(250×4.6mm,5μm)chromatographic column;mobile phase was acetonitrile-0.4%phosphoric acid(8:92);column temperature was 30℃;the flow rate of 1.0ml/min;detection wave length of 327nm.The average content of chlorogenic acid in BIMINTING Granule is 4.50mg/g.ConclusionThis study carried out qualitative identification and content determination as well,and set up quality standards to ensure the good quality of the granule.