Study On Extraction Technology Of Dengyinnaotong Capsule And Improvement Of Quality Standard

Objective:Determine the extraction process of Dengyinnaotong capsules and prepare the finished products under this technological condition;use the prepared finished capsules to conduct quality research such as identification,fingerprinting,and content determination,which provides important for the quality control of Dengyinnaotong capsules in accordance with.Methods:1.Using the extraction rate,scutellarin transfer rate,and total flavonoid content as reference indicators,the specific parameters of the concentrated liquid alcohol precipitation density,alcohol precipitation temperature,stirring time,and standing temperature during the extraction process were investigated to determine Dengyinnaotong capsule extraction process.2.Using the total number of chromatographic peaks and total peak area as reference indicators,the extraction conditions of the contents were screened from the three aspects of extraction solvent,extraction time,and content amount,so as to optimize the pretreatment method of Dengyinnaotong capsules.3.Taking Dengyinnaotong Capsule HPLC peak shape,baseline,resolution,and retention time as the reference indicators,the detection wavelength,mobile phase,gradient conditions,flow rate,column temperature,stationary phase,and injection volume are taken as reference indicators.The chromatographic conditions were screened in various aspects to determine the HPLC fingerprint of the contents of Dengyinnaotong Capsules.4.Through the method of comparing the retention time of the reference substance under the same chromatographic conditions,identify some common peaks in the HPLC fingerprint.5.Based on the chromatographic conditions of the HPLC fingerprint,the HPLC method is used to detect the content of wild baicalin and verify the methodology.6.The content of total flavonoids was determined by ultraviolet spectrophotometry and the methodology was verified.Results:1.Determine the process parameters in the extraction process as the concentration of concentrated liquid alcohol precipitation density 1.10-1.20(not included),alcohol precipitation temperature40℃,stirring time 1h,standing temperature30℃.2.Established a thin-layer identification method for the four medicinal materials in the Dengyinnaotong capsule prescription,and conducted a durability test on the identification method,with good results.3.Determine the pre-treatment ultrasonic extraction method as methanol extraction,extraction for 30 minutes,and the amount of content 0.2g.4.Established Dengyinnaotong Capsule HPLC fingerprint and selected 10 common peaks as characteristic peaks;HPLC fingerprint chromatographic conditions:COSMOSIL C18(4.6mmx250mm,5nm)as stationary phase,acetonitrile(A)-0.12%(V/v)Phosphoric acid aqueous solution(B)is the mobile phase,column temperature is 40℃,flow rate is 1.0ml/min,injection volume is 10μl,gradient conditions are 0-2min,5%A-5%A;2-5min,5%A-10%A;5-20min,10%A-17%A;20-45min,17%A-17%A;45-55min,17%A-25%A;55-75min,25%A-55%A;75-80min,55%A-55%A.5.By comparing the retention time of the reference substance under the same chromatographic conditions,five common peaks are identified;peak 1 is chlorogenic acid,peak 2 is scutellarin,peak 4 is 3,4-dicaffeoylquinic acid,peak 7 is 4,5-dicaffeoylquinic acid,peak 10 is apigenin.6.The content of wild baicalin was determined under the chromatographic conditions of the HPLC fingerprint,and the method verification results met the requirements.7.Ultraviolet spectrophotometry was used to determine the content of total flavonoids,and the method verification results met the requirements.Conclusion:Studies have shown that the extraction process of Dengyinnaotong capsules is stable and feasible,and the quality is controllable;the quality can be controlled through the preliminary quality standard(draft),and the quality standard control can be improved.