Studies On Preparation Process And Quality Standard Of Di Shao Compound Granules

Objective: To study the preparation technology,quality standard and primary stability of compound Dishao granule,and to provide the theoretical basis for preparing safe,effective and stable compound Dishao granule.Methods:(1)The single factor and Box-Behken experimental design were used to optimize the water extraction process parameters of four herbs,including catalpol.(2)The single factor and star point-response surface methodology were used to optimize the ethanol extraction parameters of the four herbaceous peony,Paeonia lactiflora,and Eucommia ulmoides Oliv,With the yield of paeoniflorin,chlorogenic acid and ethanol extract as indexes.(3)The single factor and orthogonal experiment design was adopted to optimize the forming process of granule,taking shape,hygroscopicity and angle of repose as index.(4)To study the thin layer identification method of Radix Rehmanniae,Radix Paeoniae Alba,Eucommia,and the physical and chemical identification method of the raw keel,and establish HPLC content of catalpol,paeoniflorin and chlorogenic acid test methods.(5)The preliminary stability of the granules was studied,and the stability of the granules was investigated for 6 months.The stability of the granules was investigated for 3 months,and the properties of the granules,the identification and the content determination were investigated.Results:(1)Determine the best water extraction process for 12 times the amount of water,extracted 3 times,each time 30 min.(2)The optimum extraction conditions were as follows: ethanol volume fraction 60%,extraction time 60 min,ratio of material to liquid 11 times,extraction 2 times.(3)The optimal molding process was determined by mixing 7: 3 mixture of compound Dao Shao powder with dextrin,90% ethanol as wetting agent,and adding 20% of extract powder into granules.(4)The contents of catalpol,paeoniflorin and chlorogenic acid in the preparations were determined by high performance liquid chromatography(HPLC),and the contents of catalpol,paeoniflorin and chlorogenic acid in the preparations were determined by TLC,The mobile phase consisted of acetonitrile-water(0.5: 99.5)and methanol: 0.3% glacial acetic acid water gradient elution,0 ~ 12 min: 20:80,12 ~ 20 min: 30:70,detection wavelength 210 nm,230 nm and 327 nm,flow rate: 1 mL/min;column temperature: 25℃;injection volume: 10 μL.(5)stability of granules: the above indicators in 6 months were not significantly changed,indicating that the stability of the preparation is better.Conclusion: The preparation process is reasonable and feasible,the quality standard is simple,rapid and accurate,and the quality of the finished product is stable.