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一种新型杜仲冲剂的生产工艺研究

Processing Technology of a Noval Infusion from Eucommia Ulmoides Leaves

【作者】 郭莹

【导师】 尉芹;

【作者基本信息】 西北农林科技大学 , 林产化学加工工程, 2011, 硕士

【摘要】 杜仲(Eucommia ulmiodes Oliv.)为单属科单种属植物,其皮和叶中含有多种药用成分,如绿原酸、黄酮、桃叶珊瑚苷,多种维生素、氨基酸,丰富的矿物质铁、钙、钾、锌、镁、硒等天然植物微量元素,具有调节血压、血脂和血糖,抗氧化、抗衰老及抗肿瘤,增强免疫力,减肥美容等保健作用。本研究对杜仲有效成分提取工艺进行了深入的研究,优化了提取工艺,提取出了富含生物活性物质的浸膏。在此基础上,研究了杜仲冲剂的造粒工艺,为新型杜仲保健品和药品的开发提供理论依据。研究结果如下:一、杜仲叶有效成分提取工艺以杜仲叶中的生物活性物质绿原酸和总黄酮为指标,利用响应面法优化提取杜仲叶中的工艺参数。在分析单因素的基础上,以绿原酸和总黄酮的得率为响应值,以乙醇浓度(%)、提取温度(℃)、提取时间(h)、料液比为考察因素,并采用响应面设计实验方法优化提取工艺,其最优条件为乙醇浓度55%、提取温度63℃、提取时间2.2h、料液比为1:13。在此条件下,绿原酸和总黄酮的得率分别达0.81%和0.51%。二、杜仲冲剂的制备工艺通过一系列的单因素试验选择不同的矫味剂、赋型剂、润湿剂,并从实际生产中常用的制粒方法湿法制粒、快速搅拌制粒、流化喷雾制粒中选择快速搅拌制粒为主要的制粒方法。以粒度不合格率为响应值,确定最佳提取工艺参数为:甜菊糖苷用量为杜仲提取物的0.78%、β-环状糊精与药粉质量之比为6,乙醇浓度为65%,乙醇用量(L)与药粉量(kg)比例为l︰6,干燥温度为70℃,在此条件下,杜仲冲剂的颗粒不合格率为仅为6.12%。通过本课题的研究,得到了完整的一套杜仲冲剂制备工艺:杜仲叶经除尘、除杂,并于105℃杀青10min后晾干,粉碎,加入55%乙醇,乙醇用量(L)与杜仲叶(kg)比例为13︰1,在63℃的温度下提取2.2 h后,在60℃下浓缩、干燥,得到杜仲提取物干粉,粉碎,加用量为杜仲提取物干粉的0.78%的甜菊糖苷、6倍于其他药粉重量的β-环状糊精、并加入浓度为65%的乙醇,乙醇用量(L)与药粉量(kg)比例为l︰6,混合均匀后,倒入快速搅拌制粒机中制粒,而后在70℃下进行干燥,时间为20 min,成型后即为杜仲冲剂。

【Abstract】 Eucommia ulmiodes Oliv. is a plant species with mono genus and family. The bark has been a traditional Chinese medicine for thousands of years. Modern scientific research has confirmed that the functional constituents in the leaf are similar to the bark. Based on this finding, the leaf has been listed in China Pharmacopoeia with therapeutic effects similar to the bark. The leaf contains a variety of medicinal ingredients, such as chlorogenic acid, flavonoids, aucubin, vitamin, amino acids, and minerals. The medical functions of the leaf include regulating blood pressure, lipids and glucose, anti-oxidation, anti-aging, anti-tumor, enhancing immunity, beautifying skin and anti-obesity.In order to make health-care products from the leaves of E. ulmoides, an experiment was conducted on the optimization of the extraction parameters of active ingredients the granulation process of the extracts which are rich in functional constituents. The results are as follows.1. Extraction of active ingredients of leaves of Eucommia ulmoidesResponse surface methodology (RSM) was employed to optimize the extraction parameters of chlorogenic acid and flavonolds from the leaves of E. ulmoides. Based on one-factor experiment, the effects of four independent variables, namely the concentration of ethanol (%) extraction temperature (°C), time (h) and the ratio of material to solvent on the extraction yields of chlorogenic acid and flavonoids were investigated, and then the response surface analysis was used to optimize conditions. The optimal extraction parameters were: ethanol concentration: 55%, extraction temperature: 63°C, time of extraction: 2.2h and material to solvent 1:13 according to the response surface analysis. Under these conditions, the extraction yields of chlorogenic acid and flavonoids were 0.81%, 0.51% respectively.2. Development of Eucommia granulesFirstly, optimal additives were screened from different flavoring agents, excipients, and wetting agents. Then preferable method of granulation was selected from three conventional methods, namely, fast stirring granulation, wet granulation, rapid mixing granulation, and fluidized spraying granulation. Failure rate of particle size was investigated and then the response surface analysis was used to optimize conditions. The optimal extraction parameters were: 0.78% stevia,β-cyclodextrin to powder: 6, 65% ethanol concentration, ratio of ethanol (L) to the powder volume (kg) 1:6, drying temperature of 70°C, in these conditions, Eucommia granules failure rate of particles size was as low as 6.12%.Based on the results mentioned above, a completed flow of making Eucommia granules were proposed as Eucommia leaf after de-dusting, cleaning, and drying 10 min at 105°C, grinding, added 55% ethanol, and the ratio of ethanol (L) to Eucommia leaf (kg) 13:1, and extracted at 63°C about 2.2h, next, concentrated and dried at 60°C. After grinding, the Eucommia leaf extract powder added 0.78% stevioside, theβ-cyclodextrin which was 6 times of the weight of other powder, then continued to add 65% ethanol, and concentration of ratio of ethanol (L) to the powder volume (kg) l:6, after mixing, granulated into the machine the rapid mixing granulation, and then dried under 70°C, 20 minutes.

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