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1、最新资料推荐分类号 学校代码 10412密 级 学 号 2008013 江西中医学院 硕士学位论文复方乌鸡片制备工艺与质量标准研究学位申请人指导教师姓名专业名称中药专业申请学位类型科学学位论文答辩日期年 月 日江西中医学院硕士学位论文原创性声明本人郑重声明:所呈交的硕士学位论文,是个人在导师的指导下,独立进行研究工作所取得的成果。除文中已经特别加以注明引用的内容外,本论文不含任何其他个人或集体已经发表或撰写过的作品成果。对本人的研究做出重要贡献的个人和集体,均已在文中以明确方式标明并致谢。本人完全意识到本声明的法律结果由本人承担。学位论文作者签名_日 期: 年 月 日关于硕士学位论文使用授权的
2、声明本人完全了解江西中医学院有关保留使用硕士学位论文的规定,同意学院保留或向国家有关部门机构送交论文的复印件和电子版,允许被查阅和借阅。本人授权江西中医学院可以将本硕士学位论文的全部或部分内容编入有关数据库进行检索。可以采用影印、缩印或其他复印手段保存和汇编本硕士学位论文。(保密论文在解密后应遵守此规定)论文作者签名_ 论文导师签名_日 期: 年 月 日中文摘要目的:复方乌鸡片由乌鸡、山药、白术、茯苓、熟地黄、牡丹皮、黄芪(蜜灸)、党参、川芎、当归、白芍(酒炒)、五味子(酒制)共十二味药精制而成,具补气血,益肝肾。临床主治妇女气血两虚或肝肾两虚的月经不调,脾虚或肾虚带下。对复方乌鸡片的制备工艺
3、、质量标准和稳定性三方面进行了研究与考察,确定了制剂工艺,质量检测指标,产品有效期,使之更适用于工业化大生产的需要,对推进药物开发战略的实施,具有重大的意义。方法:1.工艺研究1.1 提取工艺研究1.1.1乌鸡提取工艺研究以得膏率和含氮量为指标, 考察提取溶剂用量对试验结果的影响,结果确定提取溶剂用量为药材量的2倍。1.1.2山药、黄芪等药材提取工艺研究由于原提取工艺条件较为详细,因此仍沿用“复方乌鸡口服液”中药材的提取工艺,验证了相关参数。1.2 成型工艺根据片剂的制剂要求,通过对所用辅料进行筛选,确定处方及制法。制法:称取干膏混合物、微晶纤维素、低取代羟丙基纤维素混匀,用3%PVPk30乙
4、醇溶液作为粘合剂制成颗粒,60烘干,整粒,加入颗粒量1%的硬脂酸镁,混匀,压片,包薄膜衣,即得。2. 成品的质量标准研究2.1 鉴别2.1.1优化了方中牡丹皮、当归、白芍的薄层鉴别方法。2.1.2 建立了方中川芎药材的薄层鉴别方法。2.3 含量测定原制剂质量标准中,只规定了总氮量的测定,无专属性,但考虑乌鸡为处方中君药,其蛋白质经水解成为氨基酸和多肽,故本质量标准中仍保留该项测定,通过10批样品的检测结果,拟定“本品每片含氮量(N)不得少于5.5mg”。另增加了用高效液相色谱法测定方中芍药苷的含量,方法学实验表明,在以十八烷基键合硅胶为填充剂,乙腈:0.1mol/L磷酸(15:85)为流动相,
5、检测波长230nm的色谱条件下,其它成分对芍药苷无干扰,能达到基线分离,芍药苷的进样量在0.10791.0790g范围内与峰面积呈良好的线性关系,回归方程:Y=1188801X-21765,r=0.9997,3回收率为100.95%,RSD=1.39%(n=6),通过10批样品的测定结果,拟定“本品每粒含芍药苷(C23H28O11)不得少于0.85mg”。3稳定性考察对制剂进行了9个月的长期稳定性考察,表明本品内在质量稳定;6个月加速实验(温度40C2C,相对湿度75%5%),表明本品内在质量稳定。故暂定有效期为24个月。结果:1确定了复方乌鸡片的生产工艺。2建立了丹皮酚对照品;当归、川芎对照
6、药材;白芍对照药材、芍药苷对照品的薄层色谱鉴别方法。3. 首次建立了芍药苷的HPLC含量测定方法,该方法准确、快速、灵敏,可以作为复方乌鸡片的质量控制指标。讨论:1原复方乌鸡口服液含量测定只规定了总氮量的测定,无专属性,但考虑乌鸡为处方中君药,其蛋白质经水解成为氨基酸和多肽,故本质量标准中仍保留该项测定,本制剂同时以芍药苷为质控指标,采用高效液相法测定,简单易行,灵敏度高。2.复方乌鸡片的制备过程中,成型工艺很关键,实验中对处方的配比、赋形剂的选择与用量进行了考察,还有待于在今后的生产中进一步完善。3.将该产品制成片剂,使之成为具有较高生物利用度,服用携带方便的制剂,从根本上克服了原制剂的缺点
7、,基本实现了“三效、三小、五方便”的目的,同时也将创造更大的经济效益和社会效益。关键词:复方乌鸡片;芍药苷;高效液相色谱法;制备工艺;质量标准Study on the Preparation Process and Quality Standard of the Compound Wuji TabletAuthor Directed by AbstractObjectiveThe Compound Wuji Tablet consists of 12 Chinese medicine which are Gallus gallus, Dioscoreae rhizoma, Rhizoma at
8、ractylodis, Poria cocos, Radix Rehmanniae Praeparata, Cortex Moutan, Radix Astragali praeparata cum melle, Radix codonopsis, Rhizoma chuanxiong,Radix angelicae sinensis, Radix paeoniae alba(wine-processed) and Fructus schisandrae chinensis(wine-processed).It is applied mainly to benefit qi and blood
9、, and reinforce liver and kidney and mainly for the treatment of clinical womens abnormal menstruation, spleen deficiency, or morbid leukorrhea of kidney deficiency caused by the deficiency of both qi and blood or the deficiency of liver and kidney. By the study on three aspects including the prepar
10、ation process, quality standards and stabilization of the Compound Wuji Tablet, preparation process, quality inspection indexes, and the production period of validity were determined and better applied to meet the needs of the mass production which has great significance for the promotion of drug de
11、velopment.Methods:1. Process research1.1 Extraction process research1.1.1 Extraction process research of Gallus gallus With the extract yield and nitrogen content as markers and inspection of the influence on the experiment results of different amounts of extraction solvent, the amount of extraction
12、 solvent was determined, that is twice as much as the amount of the medicinal materials.1.1.2 Extraction process research of Dioscoreae rhizoma, Radix astragali praeparata cum melle etc.As the original process is relatively detailed, the extraction process continues to use the one of Compound Wuji O
13、ral Liquid for the extraction of the Chinese medicinal materials and the related parameters were verified.1.2 Study on the process of preparing dosage formBased on tablets preparation requirements, prescription and preparation process were determined by screening excipients used. Method: weigh and m
14、ix dry extract mixture, microcrystalline cellulose and L-HPC, make into particles by using 3% PVPk30 Ethanol Solution, dry at 60, dressing particles, add 1% magnesium stearate, do blending, pelleting, and film coating.2. Study on the quality standards of production2.1 Identification 2.1.1 Optimized
15、the method of thin layer identification for Cortex Moutan, Radix angelicae sinensis and Radix paeoniae alba in the prescription.2.1.2 Established the thin layer identification for Rhizoma chuanxiong in the prescription.2.2 Content determinationAs there is only the total nitrogen content determination of no specificity in the original preparation quality standard