【作者】 李晶；

【导师】 季宇彬；

【作者基本信息】 哈尔滨商业大学 ， 制药工程， 2014， 硕士

【摘要】 颠茄磺苄啶片(又名:泻利停),中的主要成分为磺胺甲噁唑、甲氧苄啶、和颠茄流浸膏,对肠杆菌科细菌、淋球菌、脑膜炎奈瑟菌、金黄色葡萄球菌等具有较好的抑菌作用,在临床上主要用来治疗因细菌、病毒等引起的慢性腹泻以及肠炎等疾病都有很好的治愈效果。本品也因副作用少,价格低廉等优势而被广泛用于临床。本文在质量标准研究方面主要对其做了定性和定量的研究。在定性方面,做了性状、鉴别、检查等研究。在定量分析方面,做了含量测定、溶出度的测定、稳定性进行系统试验,检测各县指标是能达到标准用以确定各相应的质量标准及控制标准。试验测定结果如下:(1)质量检查:首先采用化学法,鉴定结果均显示为正反应,然后又采用高效液相的方法对这两种主要成分进行鉴别:鉴定结果均显示SMZ和TMP与对照品具有相同的保留时间,用化学法对颠茄流浸膏进行鉴别,结果呈正反应。颠茄磺苄啶片的重量差异均在3%以内,符合药典规定;对本品脆碎度的考察结果:减失量均小于1%,并且无粉碎断裂的产品;崩解时限的测定结果为:崩解时间均在13min内,符合药典规定:在微生物限度的检查中,细菌、霉菌、酵母菌数均小于1Ocfu/g,大肠埃希氏杆菌未检出。(2)含量测定的结果:采用高效液相色谱法对本品中的磺胺甲噁唑和甲氧苄啶两种主要成分进行含量测定,测定结果为:甲氧苄啶在6.01μg/ml~90.15μg/ml浓度范围内,浓度与峰面积呈线性相关(r=0.998),平均加样回收率为99.53%,RSD为0.58%;磺胺甲噁唑在30.04μg/ml-450.60μg/ml浓度范围内,浓度与峰面积呈线性相关(r=0.9992),平均加样回收率为 99.97%,RSD为0.29%。(3)溶出度的测定结果:经试验,最佳溶出度的方案为:以盐酸溶液(9→1000)为溶出介质,体积为1000ml,转篮法以每分钟150转的转速进行试验,在30分钟时取样,并用0.8μm滤膜过滤样品溶液。三批供试品在30分钟溶出度均大于80%。最后得出结论:颠茄磺苄啶片在强光,高湿等条件下略有变化，但变化不明显,所以在生产过程中应尽量降低环境的湿度,以保证产品的质量。其贮藏条件定为遮光,密封,干燥处保存。故在保存药品时以注意贮藏条件。含量测定试验中采用高效液相色谱法,测定结果磺胺甲噁唑均为标示量的95.0%以上:甲氧卞啶含量均为90%以上。我们经过系统性的试验,认为本品的质量研究方法可靠,重现性好,简单易行,能控制本品的质量。在溶出度的试验中,才用转篮法用高效液相色谱法进行溶出度的测定,测定结果均大于80%。根据有关稳定性的基本要求,对注颠茄磺苄啶片的稳定性进行了考察,包括6个月加速试验考察,结果显示含景略有降低,其他各项指标均无明显变化,微生物含量限度结果符合规定。本品经长期留样12个月考察,各项指标均无明显变化。本品经6个月的加速试验及12个月的长期留样考察结果表明,各项指标均未发生明显的变化,说明颠茄磺苄啶片的稳定性良好。更多还原

【Abstract】 Belladonna Sulfamethoxazle and Trimethoprim Tablets,the main ingredient in this product is sulfamethoxazole,trimethoprim,and Belladonna liquid extract,The prod uct has a good antibacterial effect of Enterobacteriaceae,Neisseria gonorrhoeae,Neisseria meningitidis and Staphy,lococcus aureus.In the clinical treatment,it mainly used of chronic diarrhea and enteritis,which caused by bacteria,and viruses.This product is also due to fewer side effects and low cost advantage so it is widely used in clinical.This article in the preparation process maturity after the product character,identification,inspection,Traits,identification,inspection,Determination of dissolution,the content determination of the system test,to determine the appropriate quality standards and control index.The experimental results are as follows:(1)We use chemical method to identify sulfamethoxazole and trimethoprim,nd the results showed a positive reaction,then we using the HPLC method for the identification of these two main components,the results showed SMZ,TMP and reference have the same retention time.Chemical method Belladonna liquid extract were identified,the results showed a positive reaction.the weight difference of Belladonna sulfur Trimethoprim Tablets are within 3%,in line with Pharmacopoeia.the results of the friability of the product:The product is less than 1%loss of volume,and no ground breaking products;Disintegration time measurement results is:disintegration timeaveragein3min,in line with Pharmacopoeia;Microbiall imit check,bacteria,fungi,yeast count of less than10cfu/g,Escherichiacoli was not detected.(2)Determination results:HPLC method for simultaneous determination of trimethoprim and sulfamethoxazole,Linear least-square regression analysis of the calibration graph demonstrated linearity between the response(peak area)and the nominal concentrations of TMP(6.01μg/ml~90.15μg/ml)r-0.9998 and SMX(30.04μg/ml~450.6μg/ml)r=0.9992(3)The measurement results of the dissolution:After testing the best solution dissolution is:Hydrochloric acid solution(9 1000)as the dissolution medium,volume of 1000ml,basket method at 150 revolutions per minute test speed,sampling time30 minutes and treated with 0.8μm membrane filter sample solution.In three batches of 30 minutes for the dissolution of the sample of greater than 80%.Conclusion:This product is a slight change in bright light,humidity and other conditions,but did not change significantly,Therefore,in the production process should be to minimize the humidity,to ensure product quality.Its storage conditions is shading,sealed,dry place,therefore,when saving drugs we should pay attention to storage conditions Determination by HPLC test,measurement results were greater than90.0%.We go through a systematic test,believe that the quality of the product research method is reliable,reproducible,and simple,can control the quality of the product.Dissolution of the trial,only with rotating basket method were determined by HPLC dissolution,the measured results were greater than80%.According to the basic requirements for stability,the stability of the belladonna sulfonamide trimethoprim tablets were investigated,including six months accelerated testing study,the results showed that the content decreased slightly,other indicators did not change significantly,microbiological limits results of compliance.This product is by a long-term study stay like 12 months,the index did not change significantly.This product was accelerated testsixmonthsandl2months of long-term stay kind study results show that the indicators were not changed significantly,indicating good stability belladonna sulfonamide trimethoprim tablets.更多还原