【作者】 刘军凯；

【导师】 安莲英；

【作者基本信息】 成都理工大学 ， 分析化学， 2007， 硕士

【摘要】 肝乐宁胶囊是基于成都中医药大学张廷模教授提供的临床经验方研制而成。包括郁金、茵陈和白术等药，主要用于治疗高发病率的脂肪肝人群。本研究以处方药物的化学成分与性质和药理作用为依据，对肝乐宁胶囊制备工艺和质量控制方法进行研究，系统地优化了醇提和水蒸气蒸馏及包合、除杂、浓缩干燥、成型等制备工艺的条件，为开发疗效确切的治疗脂肪肝的中药六类新药奠定了基础。以姜黄素含量及干膏率为考察指标，实验优化郁金药材中姜黄素的提取条件为60％乙醇回流，15倍药材溶剂量，提取时间1h，温度80℃，单次提取，姜黄素的提取量达1.119mg／g_生药；采用S-8树脂纯化郁金提取液，实验优化纯化条件为：上柱液pH=6，吸附流速为2BV／h，吸附率达97.12％。树脂解析工艺条件为：用pH为6的80％的乙醇为洗脱剂，控制流速为3BV／h，解脱率为95.55％。树脂纯化过程姜黄素的保留率达到90％以上，干膏率由纯化前的7.85％降为2.47％，干膏中姜黄素含量由纯化前的1.42％提高到4.48％。以6，7-二甲氧基香豆素（DEM）、挥发油含量及干膏率等指标，实验优化水蒸气蒸馏法提取茵陈、白术挥发油的条件为：12倍水量，浸泡12h，蒸馏6h，平均提取挥发油量为0.79ml／250g_生药；采用75％乙醇对水蒸馏得到的水煎液沉淀分离，DEM的保留率为99.5％，干膏率由15.7％降低为2.1％。β-环糊精包合茵陈、白术挥发油的工艺条件为：茵陈、白术挥发油与β-环糊精投料比为1∶10，β-环糊精与加水量的比为1∶10，包合时间为2.5h，挥发油包结率达81.6％。采用低温减压旋转蒸发浓缩纯化后的郁金和茵陈、白术提取液，姜黄素和DEM的损失率分别为5.5％和3.7％。采用冷冻干燥法干燥清膏，姜黄素和DEM的损失率分别为3.7％和1.4％。优选成型主要工艺条件为：浸膏粉与可溶性淀粉的配比为8∶2，以95％浓度的乙醇润湿，其用量为40ml／100g_浸膏，成型颗粒的合格率不少于80％。总制备工艺中姜黄素、DEM和总挥发油的转移率分别为81.8％、78.6％、72.5％，实验的RSD≤3.56％（n均为3）。参照药典，对实验药材及制得的胶囊内容物进行了薄层鉴别，对照药材和供试品在相应位置均有相同颜色的斑点；选用高效液相色谱法和双波长扫描法测定制剂中姜黄素和DEM的含量各为1.846mg／g_颗粒、7.944mg／g_颗粒。更多还原

【Abstract】 Ganlening capsule is based on the Chengdu University of Traditional Chinese Medicine Professor Zhang for the clinical experience to develop into a modern Chinese proprietary, including Curcuma Louga L., Artemisia capillariea Thunb. and Atractylodes macrocephala koiz, mainly for the treatment of high incidence of fatty liver crowd. In this study, prescription drugs and the chemical constituents of nature and based on the pharmacological effects, the capsule Ganlening Preparation and major quality-control, identified Ganlening capsules preparation line, and the main technology index components, optimized conditions of preparation, which included refluxing extraction, water decocting extraction, purification, steam distillation, packing procedure, condensing and drying process, granulation by the numbers, study for the development of the exact efficacy of the treatment of fatty liver medicine six new drugs lay the groundwork study。Guided by the content of curcumin and paste rate, screening tests, identified Curcuma Louga L. the extraction and purification technology line. Curcuma Louga L. curcumin optimize the extraction conditions is 60 % ethanol, 80℃,15 times of materials, time of extraction is an hour, single extraction, curcumin extraction to1.119mg/g pharmacognostic. Using resin purification Curcuma Louga L. extract liquor, guided by the content of curcumin and paste rate, find that resin S-8 is better. The optimal conditions for the resin purification: the pH of liquid is 6, velocity of flow is 2 BV/h and at room temperature, adsorption rate is 97.12%. Resin analytic process conditions: pH=6, 80 % ethanol solution eluant, control flow rate of 3 BV/h, extrication rate is 95.55 %. Under these conditions, column purification process of curcumin retention rate of over 90 %. the percentage of the extract reduced to 7.85 % from 2.47 %, the purity of product reached 4.48 %. Dry extract purified curcumin content from 1.42% up to 4.48%.Guided by 6,7-dimethoxycoumarin(DEM), volatile oil content and the rate of dry extract, the optimum conditions of steam distillation extraction volatile oil from Artemisia capillariea Thunb. and Atractylodes macrocephala koiz is: 12 times water, soak for 12 hours distillation every six hours, on average for the extraction of volatile oil is 0.79 ml/250 g pharmacognostic; through the use of 75 % ethanol edulcoration the distillation of the water decoction, dry extract to reduce the rate from 15.7 % to 2.1%. The proportion of volatile oil andβ-cyclodextrin was 1:10, the proportion ofβ-cyclodextrin and water was 1:10, inclusion time was 2.5 h, inclusion rate was 81.6%.Concentrated in the drying process, using low-temperature rotary vacuum evaporator to concentrate purified extract of Curcuma Louga L. and purification of Artemisia capillariea Thunb. and Atractylodes macrocephala koiz decoction, DEM content and the content of curcumin loss rate of 3.7 % and 5.5 %, using freeze-drying dessicate DEM and curcumin content and the loss rate of 1.4 % and 3.7 %.In molding process optimization of the main conditions: extract soluble starch powder and the ratio of 8:2, 95 % ethanol concentration of wetting, dosage of the extract powder 40 ml/100 g creat extract. Forming particles passing rate of not less than 80%.In the optimum preparation, the transfer rate of curcumin, DEM and volatile oil reached 81.8 %, 78.6 %, 72.5 %, respectively, and RSD≤3.56 % (n=3) in their reduplicate experiments.Pharmacopoeia reference to experimental medicines and the capsule system of TLC and HPLC, dual wavelength determination, In Curcuma Louga L., Artemisia capillariea Thunb. and Atractylodes macrocephala koiz ingredients of TLC, medicines for the control sample and the corresponding position is the same color spots, and the color clear, no negative interference; use dual-wavelength scanning method to detect the effects of curcumin and DEM content, the curcumin and DEM content in the granuleis 1.846 mg/g granule, 7.944 mg/g granule.更多还原