【作者】 李蕊；

【导师】 张秀英；

【作者基本信息】 东北农业大学 ， 基础兽医学， 2008， 硕士

【摘要】 中药透皮剂是由东北农业大学药理教研室根据传统中医理论并结合现代制剂工艺研制而成的中药复方制剂,由黄芩、蒲公英、连翘等中药组成,具有清热解毒、抗菌消炎、消肿止痛、活血通乳的功效。临床上主要用于治疗各种原因引起的临床型乳房炎。根据新兽药管理条例,本试验研究了中药透皮剂的质量控制方法,起草了中药透皮剂的质量标准草案,研究结果为新兽药的申报及其质量控制和规范化生产提供了保障。在性状方面,主要描述了中药透皮剂的颜色和外观性状,本品为黄褐色、均匀细腻的软膏,且在贮藏过程中性状不发生变化。在定性鉴别方面,采用薄层色谱法(TLC)对处方中主要的三味药材分别进行了定性鉴别。黄芩:采用聚酰胺薄膜,以36%乙酸为展开剂,以2%三氯化铁乙醇溶液为显色剂,日光下检视。蒲公英:采用硅胶G薄层板,以乙酸乙酯-甲酸-水(7﹕2.5﹕2.5)的上层溶液为展开剂,置紫外光灯(365nm)下检视。连翘:采用以0.5%羧甲基纤维素钠为黏合剂的硅胶G薄层板,以氯仿-甲醇(5﹕1)为展开剂,以10%硫酸乙醇溶液为显色剂,105℃烘烤至斑点显色清晰。结果表明,供试品在与对照品和对照药材相应的位置上显相同颜色的斑点或荧光斑点,阴性对照无干扰,斑点分离效果好,证明所选方法的专属性强。在含量测定方面,采用高效液相色谱法(HPLC)同时测定制剂中的黄芩苷和连翘苷。采用中科院大连化物所C18色谱柱(250×4.6mm,10μm),流动相:乙腈(A)-0.002%磷酸溶液(B)(A+B=100%)作梯度洗脱,检测波长280nm,流速1.0mL·min-1,柱温25℃。结果表明:黄芩苷和连翘苷在10μg·mL-1～80μg·mL-1范围内峰面积与药物浓度呈良好的线性关系,回归方程分别为Y=38561x﹣7630.3、Y=7843.7x﹣2177.1,相关系数分别为r2=0.9994、r2=0.9995,平均回收率分别为98.36%、97.60%。本试验还对透皮促渗剂氮酮的含量进行了测定,采用中科院大连化物所C18色谱柱(250×4.6mm,10μm),流动相:甲醇-水(85﹕15),检测波长:225nm,流速1.0mL·min-1,柱温25℃。氮酮在1mg·mL-1～5mg·mL-1范围内峰面积与药物浓度呈良好的线性关系,回归方程为Y=747896x+28788,r2=0.9991,平均回收率为98.16%。运用上述方法对5批中药透皮剂的含量进行测定,制订了主要成分的含量限度,即每克中药透皮剂中含黄芩苷和连翘苷的量不少于700μg和150μg,氮酮含量不少于3.6%。检查项目应符合《中华人民共和国兽药典》(2005年版)附录中相应的制剂通则中的规定,还应根据中药透皮剂的特性、工艺及稳定性考察结果,制订其他的检查项目。本试验对3批中药透皮剂的透皮量、乳化稳定性、装量差异、微生物限度、重金属和砷盐进行了检查。结果表明,3批样品均符合兽药典的相应规定。本试验对3批制剂进行了加速试验和长期试验。结果表明,中药透皮剂的稳定性良好,室温下保质期可暂定为2年。更多还原

【Abstract】 According to the traditional Chinese medical theory and the modern preparing process,the northeast agriculture university pharmaco-laboratory developed the traditional Chinese medicine percutaneous oinment,which was composed of Scutellaria,Dandelion and Weeping Forsythia Capsule, its functions were heat-clearing and detoxicating、bacteriostasis and dephlogisticate、detumescence and odynolysis、promoting blood flow and lactogenesis.It was mainly used to treat mastitis which had clinical symptom and the mastitis caused by all kinds of reasons. According to the new veterinary drugs management regulation,the experiment studied quality control methods of the traditional Chinese medicine percutaneous oinment,established quality criteria protocol,the results provided the assurance for the report to a higher authority of the new veterinary drugs and the normalization production.About its characters,we mainly described its color and appearance,it was yellow brown、uniform and exquisite oinment,its characters did not change in store.Using the thin-layer chromatography(TLC) to identified three medicinal materials in the prescription.Baicalin:a polyamide film was adopted with developing solvent 36% acetic acid, alcohol solution of chloride ferric(2%) was used as colouring agent,inspected under the sunlight.Caffeic acid:a silica ged G plate was adopted with developing solvent consist of the upper layer of the mixture acetidin, formic acid and water(7﹕2.5﹕2.5),inspected at 365nm. Forsythin:a silica gel G plate which contain 0.5%CMC-Na was adopted with developing solvent consisted of chloroform and methanol(5﹕1),alcohol solution of sulfuric acid(10%)was used as colouring agent,baked it until coloration clearly at 105℃.The study indicated that the sample displayed the same spots or fluorescence spots as the control article and the control medical material did in the Chromatography,while the negative sample did not,the separation of the spots was apparent,all of these proved that the method had a higher specificity.About its assaying,the high performance liquid chromatogrophy (HPLC)method was established to determine baicalin and forsythin in the preparation.Chinese Acadamy of Science dalian Chemical research institute C18 column(250×4.6mm , 10μm)was used,the mobile phase:acetonitrile(A)-0.002% orthophosphoric acid solution (B)(A+B=100%) gradient elution, wavelength:280nm,velocity of flow:1.0ml·min-1,temperature 25℃.The results suggested that the linear ranges of baicalin and forsythin was 10μg·mL-1～80μg·mL-1,regression equations were Y=38561x﹣7630.3、Y=7843.7x﹣2177.1 respectively, coefficient correlations were r2=0.9994、r2=0.9995 respectively, average recovery were 98.36%、97.60%. In addition,we also detected azone, Chinese Acadamy of Science dalian Chemical research institute C18 column(250×4.6mm,10μm)was used,the mobile phase: methanol-water(85﹕ 15), wavelength:225nm,velocity of flow:1.0ml·min-1,temperature 25℃.The linear ranges of azone was 1mg·mL-1～5mg·mL-1,regression equations was Y=747896x+28788, coefficient correlations was r2=0.9991 average recovery were 98.16%.The methods were used to determin 5 groups of samples ,we established the main component’s content limit,baicalin and forsythin no less that 700μg and 150μg per g, azone no less than 3.6%.According to“Chinese Veterinary Pharmacopoeia”(2005) preparation general information,we also needed to work out other inspection items according to its characteristics、technology、the results of stability.we examined three group of samples,including accumulative permeation quantity,emulsive stability,content uniformity and microbial limit,and inspected the heavy metal and arsenic salt.The results suggested that the three groups of samples conform to the regulation.According to the“Stability test requests for the new Chinese traditional medicine”,oinment stability examination items.Accelerated test and long test run were carried out.The results suggested that its stability is well,and the storage life can tentatively set on two years.更多还原