The Study On Extraction Of Datura Metell And Preparation Of Atropine Sulfate From Waste Liquid

Purpose:(1)It is to optimize extraction and purification process of total alkaloid for datura metel.(2)It is to optimize preparation of atropine sulfate for mother liquor after process of preparation of Scopolamine Hydrobromid,to establish monitoring method of intermediate for industrial production of atropine sulfate and to reduce production costs and improve economic efficiency of enterprises.Method:(1)Using acid dye-UV spectrophotometry to establish the content determination of total alkaloid of datura metel.,Use the extraction rate of total alkaloid as index to optimize the best formulation.Use ethanol content,extraction time,solvent volume as influencing factor and the extraction rate of total alkaloid as index to test optimization process of datura metel by the central composite design-response surface method,which is for select the best preparation technology.(2)Through the thin layer of diluted 10 times contrast method to set up the quality control standard of intermediates Ⅰ.It is to establish by rotation method ofquality quality control standards of intermediates Ⅱ.(3)It is to establish a methods of content of atropine of intermediatesⅢby HPLC.Through single factor method and orthogonal design method combined with to optimize the process of preparation of atropine sulfat from the waste liquid after the preparation of scopolamine hydrobromidefrom datura flower,which include process of despun of the intermediate Ⅰ,process of recrystallization of intermediates Ⅱ,process of process by activated carbon,process of salifying and recrystallization of atropine sulfate.Result:(1)Compared with immersion method and ultrasonic extraction method,the extraction rate of reflux extraction is higher and the extraction time is shorter.Factors and orthogonal optimization to be 14 times 76% ethanol extracts of twice,every 160 minutes,the extraction rate of 87.61%.(2)The best separation conditions of Intermediate Ⅰof TLC is:developer: acetate-methanol-strong ammonia solution(17:2:1),reference solution spotting amount 2ul and the test solution spotting amount 2μL,reagent: Wagner’s reagent solution.saturated time for 15 min.The eligibility criteriaof Intermediate Ⅰwas which the spots of Scopolamine of sample solution of high concentration are smaller,lighter of color than the spots of Hyoscyamine of low concentration.The eligibility criteriaof Intermediate Ⅱwas the optical rotations in a 0.3 °-0.06 °(0.1 g/ml).(3)Process of despun of Intermediate Ⅰoptimizate to racemic temperature is 95 ℃,racemization time is 3.5 h-7 h.technology of recrystallization of Intermediates Ⅱ optimizate to using acetone as the solvent,heating temperature of 57 ℃,liquid ratio of 10:9 and crystallization temperature of 5 ℃,the crystallization time of 24 h.Process of decolorization of activated carbon was optimized as the activated carbon amount of 5.3%(m/V),and the decolorization time of40 min.process of salifying and recrystallization of atropine sulfate was optimized as acetone material liquid crystal than 1:6,crystallization temperature of 5 ℃,the crystallization time of 24 h.Conclusion:The preparation process of datura metel and atropine sulfate for mother liquor was stable,reasonable and feasible.The established quality standard for intermediate was stable and controllable..The research basically achieves the expected purpose.