【作者】 汪兰芳；

【导师】 韩建伟；

【作者基本信息】 湖北中医药大学 ， 中药学， 2011， 硕士

【摘要】 目的：对复方交泰巴布剂制备工艺及其质量分析进行研究,试图研制一种敷贴穴位、对失眠具有良好辅助治疗效果的外用巴布剂制剂。方法：1提取工艺研究：①肉桂挥发油提取工艺研究：采用水蒸气蒸馏法提取,以挥发油提取量为考察指标,选择浸泡时间、加水量、粉碎粒度、提取时间为影响因素,通过L9(34)正交试验优选提取工艺条件；②黄连的乙醇回流提取工艺研究：以黄连生物碱提取量为考察指标,采用紫外分光光度法测定生物碱含量,选择乙醇浓度、溶剂用量、提取时间、提取次数为影响因素,通过L9(34)正交试验优选处方中黄连药材的乙醇回流提取工艺条件。③黄连、肉桂等药材的不同提取工艺比较研究：以黄连生物碱提取量或肉桂挥发油提取量为考察指标,对黄连、肉桂等进行水提,醇提,分提,合提的比较研究,选择合适的提取工艺。2复方交泰巴布剂成型工艺研究：经预试验及资料的查阅,确定基质的种类及用量范围,以外观、初黏力、膜残留量为评价指标,采用L,8(37)正交试验对复方交泰巴布剂的基质组成进行优选。3复方交泰巴布剂质量分析研究：采用薄层色谱法对制剂中肉桂药材进行鉴别；依据中国药典中相关规定,对制剂的含膏量、初黏力、重量差异、赋型性、耐热性进行检查；制定制剂中盐酸小檗碱含量HPLC测定方法。测定色谱条件为：色谱柱：ZORBAX SB柱(250mm×4.6 mm,5μm),流动相：乙腈-0.05mol/L磷酸二氢钾溶液(35：65)(每100ml中加十二烷基硫酸钠0.4g,再以磷酸调节pH值为4.0)；检测波长为345nm；流速：1.0ml·min-1。结果：1提取工艺研究：①优选的肉桂挥发油提取工艺条件为：取10-30目肉桂药材,加8倍量水,浸泡2h,然后提取4h；②优选的黄连乙醇回流提取工艺条件为：药材加4倍量50%乙醇,提取3次,每次提取2小时。3批验证试验黄连中盐酸小檗碱的平均提取率为8.4%。③黄连肉桂等药材的不同提取工艺比较研究结果：肉桂单独水蒸气提取挥发油,收集水提取液,黄连与珍珠母合并以50%乙醇提取为最优工艺。2优选复方交泰巴布剂的基质组成为：浸膏量-聚丙烯酸钠-甘油-氢氧化铝-微晶纤维素-柠檬酸-蒸馏水=0.9：1.5：5：0.05：1：0.2：20。3复方交泰巴布剂质量分析研究：制剂中肉桂药材的薄层色谱鉴别方法简单,图谱清晰,阴性对照无干扰。制剂的含膏量、初黏力、重量差异、赋型性、耐热性符合中国药典规定。制剂中盐酸小檗碱含量测定结果显示：线性范围为0.02μg～0.2μg(r=0.9998)；稳定性试验：RSD为0.87%；重复性试验：盐酸小檗碱平均含量为0.7252%(RSD=1.53%)；平均加样回收率为97.31%(RSD=1.26%)；3批制剂中盐酸小檗碱含量分别为39.52mg/贴、38.80mg/贴、40.25mg/贴。结论：通过较系统的提取工艺、制剂成型工艺、质量分析等研究,为复方交泰巴布剂的制备开发奠定了良好的基础。更多还原

【Abstract】 Objective:To study on preparation technology and quality analysis of Fufangjiaotai Cataplasmate, attempt to develop one kind of cataplasmate which can be adhered on the acupoint to treat insomnia auxiliarily.Methods:1 The extraction technology research:①The extraction technology research of volatile oil in Cinnamomi Cortex:To optimize the conditions of extraction technology of volatile oil by wet distillation method, the L9 (34) orthogonal design experiments were carried out, in which four influence factors such as soaking time, amount of water, the size of Cinnamomi Cortex and the time of extraction were selected, and the rate of volatile oil extracted was regarded as the evaluating indices.②To optimize the extraction conditions of the ethanol reflux extraction for Coptis, the L9 (34) orthogonal design experiments were carried out, in which four influence factors such as concentration of alcohol, volume of solvent,time for extraction,number of times for extraction were selected, and the extracted yield of berberine alkaloids determined by UV was regarded as the evaluating indices.③contrast research of different extraction technology for Coptis and Cinnamomi Cortex: to select appropriate extraction technology,a comparative research was carried out among the reflux extraction the ethanol reflux extraction、extraction apart and extraction together for Coptis or Cinnamomi Cortex, in which the extracted yield of berberine alkaloids or the rate of volatile oil was regarded as the evaluating indices.2 The preparation technology research of Fufangjiaotai Cataplasmate: according to the results of preliminary test and large amounts of data,the kinds and dosages rang of excipients were determind, the proportion of the base material was optimized by the L48 (37) orthogonal design experiments, in which appearance, prelimilary adhesion and residual amount on the polyethylene membrane were as their evaluating indices.3 The quality analysis research of Fufangjiaotai Cataplasmate:It was identified for Cinnamon by TLC. According to related regulations in China Pharmacopoeia, mastic amount, adhesive ability、weight difference、bestows on the shape and heat resisting property was detected.Draft a method how the contents of Berberine in preparation was detected by HPLC.The chromatography conditions of determination were that the ZORBAX SB-C18 (4.6mm×250mm,5μm)column was used,the mobile phase was composed of acetonitrile- 0.05mol/L Potassium dihydrogen phosphate (0.4g sodium lauryl sulfate Per 100ml,adjust the PH to 4.0 with phosphoric acid solution) (35:65), the wavelength of detection is 345 nanometer, the flow rate is 1.0mL·min-1.Results:1 The extraction technology research:①The optimum conditions for the extraction technology of volatile oil for Cinnamomi cortex were that the size of medicinal material was between 10 mu and 30 mu, the amount of water was 8 times of medicinal materials, the soaking time was 2 hours, and extraction time was 4 hours.②The optimum technological conditions of the ethanol reflux extraction for Coptis,were that the medicinal materials were extracted with 4 times of 50% alcohol for three times, every time for 2 hours. The average extraction rate of berberine alkaloids in 3 batches of samples was 8.4 %.③Contrast research results of different extraction technology for Coptis and Cinnamomi:extract volatile oil from Cinnamomi apart by wet distillation method,then collect the solution extracted by water, while Coptis and Margaritiferaconcha was extracted together by the ethanol of 50%.2 The optimum proportion of the base material of the Fufangjiaotai Cataplasmata were:the mastic amount - sodium polyacrylate - glycerin-aluminium hydroxide - microcrystalline cellulose -citric acid-distilled water was 0.9:1.5:5:0.05:1:0.2:20.3 The quality analysis research of Fufangjiaotai Cataplasmate:It was very simple to identify Cinnamomi cortex in Fufangjiaotai Cataplasmate by TLC, the spots were clear, the negative contrasts were not disturbed.The mastic amount,Adhesion, bestows on the shape, heat resisting property and weight difference were in accordance with the regulations of China Pharmacopoeia.The detection of berberine alkaloids showed that their linear rang were 0.02μg～0.2μg (r=0.9998), stability (RSD) were 0.87%, average content of berberine alkaloids were 0.7252%(RSD 1.53%) in the reproducibility experiments, average recovery were 97.31%(RSD1.26%).The contents of berberine alkaloids in three batches of were 39.52mg,38.80mg,40.25mg, per patch, respectively.Conclusions:by studying on the extraction technology, preparation technology, quality analysis research, a good foundation had been laid for the further development of Fufangjiaotai Cataplasmate.更多还原