| Objective:Zhongfengtongluo Pian(a pill for stroke)is an internal product of 303 Hospital of People’s Liberation Army.It including Ephedra,Securidaca inappendiculat Hassk,Warthworm,Pinellia,Ichnocarpus Oliganthous,prepared Nux Vomica,Gardenia,Astragalus.The preparation for the treatment of stroke recovery of wind phlegm and blood stasis syndrome,symptoms as dizzy,distortion of commissure,paralalia,hemiplegia,limb numbness,tongue dark or pale,moss white and greasy,slippery pulse string.In order to have better control of the product quality of Zhongfengtongluo Pian and ensure its clinical curative effect,this research will select the optimum of extraction technology with medical materials,establish more comprehensive quality standards for this preparation;moreover,to carry out an experiment on preliminary stability for the preparations of further research and industral production.Methods:Through the orthogonal designed experiments optimizated the optimum extraction process of this preparation;Thin layer chromatography(TLC)is used for the qualitative identification of Ephedra,Securidaca inappendiculat Hassk,Ichnocarpus Oliganthous,prepared Nux Vomica,Gardenia,Astragalus and HPLC is used for determination of the content of Ephedrine,Strychnine and Brucine.The chromatographic conditions for determining the content of Ephedrine is:chromatographic column:WondaSil column(C18,250×4.6mm,5μm);the column temperature:25℃;the mobile phase:methanol-water emulsion of containing 0.1%phosphorica cid and 0.1%triethylamine(4:96);flow speed is:1.0mL/min;the wavelength detection is:210nm;sample size:10μL.The chromatographic conditions for determining the content of Strychnine and Brucine are:chromatographic column:WondaSil column(C18,250×4.6mm,5μm);the column temperature:25℃;the mobile phase:methanol-water emulsion of the same amount of O.Olmol/L heptane sulfonate and 0.02mol/L potassium dihydrogen phosphate(use 10%phosphorica cid adjust pH to 2.8)(21:79);flow speed:1.0mL/min;the wavelength detection:260nm;sample size:10μL.Methodological investigations are also carried out on both of them respectively;The preparation for inspection include:tablet weight difference,Disintegration,Microbial Limit,Heavy Metal,Arsenic salt and stability test(including accelerating and long-term experiment).Results:The optimum extraction process for the prescription was confirmed;Qualitative identification:The spots of TLC chromatogram of four kinds of Chinese herbal medicine namely Ephedra,Securidaca inappendiculat Hassk,Ichnocarpus Oliganthous,prepared Nux Vomica,Gardenia are clear,same color sports are found at the same place of testing sample in comparision with original one,no negative interference;Determination of content:Within the sample size range of 10.5～126.0μg/mL,Ephedrine Hydrocholido reference sample has good linear relationship,r=0.9997,the average recovery rate is 100.3%,RSD is 1.12%;within the sample size range of 2.50～30.0μg/mL and 1.25～20.0μg/mL,Strychnine and Brucine reference sample have good linear relationship,r=0.9999,0.9994,the average recovery rate is 100.1%,98.3%,RSD is 1.82%,1.52%.In the sample,the average content of Ephedrine Hydrocholido(C10H15NO·HCl)in every tablet is 1.28～1.62mg and the average content of Strychnine(C21H55N2O2)and Brucine(C23H26N2O4)in every tablet is 0.418～0.519mg and 0.188～0.410mg in this product respectively.The Ephedrine Hydrocholido(C10H15NO·HCl)was required no less than 1.0mg/tablet;Strychnine(C21H55N2O2)was required in 0.39～0.55mg/tablet and Brucine(C23H26N2O4)no less than 0.15 mg/tablet;Preparation of items inspected were compliance with the relevant provisions;The experiment on preliminary stability showed that the prepation was stable.Conclusion:Optimized extraction technology of Zhongfengtongluo Pian is stable and reasonable;Methodological investigations research indicates:this method are simple,accurate,sensitive,good reproducibility,and no negative interference;it can be used as the quality standard for the product;The preliminary was stable in test period. |
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