The Study Of Preparation Process And Quality Standard Of Kouyangqing Pellets

ObjectiveTo develop a clinical prescription for Recurrent Oral Ulcer into a new drug,following the guiding principle of drug registration management measures and new drug development of Traditional Chinese Medicine(TCM)and using TCM modernization technology,the preparation process and the quality standard of Kouyangqing Pellet were studied.It could provide preclinical pharmaceutical research data and lay the foundation for the study of the new drug.Methods1.Extraction and purification technologyThe comprehensive assessment criteria were the transfer rate of baicalin or berberine hydrochloride and dry ointment yield.Influence factors of the extraction process,such as soak time for herbs,solvent amount,time of process,extraction times and alcohol concentration,were researched in order to determine the optimal extraction process conditions,combining the single factor test and orthogonal test.Reduced pressure concentration and vacuum drying were used to process the extract.The different temperatures of the process,which might result from the content of index composition lower,were studied,so as to determine the optimal temperature for the process of concentration and desiccation.2.Molding processWith the assessment criteria contained yield,spherical degree and disintegration time,the influence factors,which included drug loading,wetting agent,extrusion velocity,spheronization velocity and rolling time were investigated respectively.So the composition of prescription and the optimal molding process conditions could be sure.3.Quality standardScutellaria baicalensis,Rhizoma coptidis,Radix glycyrrhizae,Radix pseudostellariae,Taraxaci herba and Dried ginger,etc in the formulation were qualitatively identified by TLC.The contents of baicalin and berberine hydrochloride were analyzed simultaneously by HPLC.The analysis of the components were performed on Inertsil ODS-3(4.6mm X 250mm,5 ?m)with acetonitrile-0.2%phosphoric acid solution(24:76)as mobile phase at a flow rate of 1.Oml/min.The detection wavelengths was at 265 nm and the column temperature was 30?.And it was inspected methodologically.Results1.Extraction and purification technologyThe optimal extraction process conditions was determined according to the orthogonal experiment:Rhizoma coptidis and Rhizoma zingiberis were extracted together with 50%alcohol for 2 times(adding 6 times amount of 50%alcohol first time,then 5 times)and 1.5 hours every time.Then filtrated and merged the filter liquor.Meanwhile other herbs were decocted with purified water for 2 times(adding 9 times amount of water first time,then 7 times)and 1 time each time.Scutellaria baicalensis was added when the water is boiling.Filtrated and merged the filter liquor likewise.The conditions of concentration and desiccation were as follows:The alcohol extract was concentrated at 60? with reduced pressure to recover the ethanol.It was the thick paste 1 and the relative density was about 1.20.Meanwhile,the water extract was concentrated at 60? with reduced pressure.It was the thick paste 2 and the relative density was about 1.20.Then the two thick pastes were merged evenly.Put the thick paste in the vacuum drying oven at 80? to dry it and until the water content below 5%.2.Molding processThe composition of prescription and the optimal molding process conditions were as follows:The powder of Kouyangqing 40%,the microcrystalline cellulose 59%and the silicon dioxide 1%,were blended,adding about 38%amount of 40%alcohol solution successively,and kneaded to the soft material.The soft material was put into the extruder,through the sieve plate(diameter 1.2 mm)at 40 r/min and made into uniform strings.Then Started the shot blasting machine,with the speed at 700 r/min,added the strings and rolling 4 minutes.Then the pellets were put in the drying oven at 50? to dry it.The 16?30 mesh cut pellets were choiced for the product.3.Quality standardIdentification:The TLC methods of Scutellaria baicalensis,Rhizoma coptidis,Radix glycyrrhizae,Radix pseudostellariae,Taraxaci herba and Rhizoma zingiberis were established.Content determination:The calibration curves showed good linearlty in the range of 12.40?185.97?g/ml with R=1 for baicalin and 3.01?45.09?g/ml with R=0.9995 for berberine hydrochloride.The average recoveries of baicalin is 99.8%and RSD was 1.02%.The average recoveries of berberine hydrochloride is 101.0%and RSD was 2.40%.ConclusionsThe studies had shown that extraction technology and molding process of Kouyangqing pellets were simple,reasonable,stable and feasible.The methods of TLC dentification and content determination were simple with exact result and good repetition and they could be used as quality standard.