【作者】 魏炜；

【导师】 银建中；

【作者基本信息】 大连理工大学 ， 安全技术及工程， 2005， 硕士

【摘要】 本文以甘草药用成分的提取、分离和纯化为目的,运用超临界CO2萃取、室温冷浸萃取以及超声波萃取等分离方法,探讨多种工艺协同作用以实现甘草资源的最大化利用。在实验研究的基础上,找到了合适的萃取、分离和纯化工艺路线和相应的技术条件,借助于现代仪器分析和检测手段,对产物进行了成分分析和鉴定。全文主要工作体现在如下几个方面:采用超临界CO2萃取甘草黄酮类物质。首先进行了单因素实验。分别对原料粒度、萃取压力、温度、CO2流量、萃取时间、以及溶胀剂选择、溶胀剂浓度、溶胀剂用量等因素进行考察,并绘制影响因素曲线。然后,在单因素研究的基础上,采用正交实验方法,进一步得出最佳萃取工艺条件。在15MPa、50℃、CO2流量18. 5mL/min条件下萃取率为7. 03%。为了获得极性物质,本文还探讨了甘草的超声波萃取和室温冷浸萃取。从萃取率、工艺条件、产物成分等技术指标出发,对上述三种方法进行比较评价。超声波萃取率为7. 72%,室温冷浸法萃取率为8. 92%。但三种方法所得产物成分各不相同。采用超声波萃取法对超临界CO2萃取后的物料进行甘草酸萃取,得到萃取率为4. 85%,使有效物质总萃取率达到11. 88%。采用薄层层析和柱层析的方法,对三种方法所得萃取物进行分离、提纯,得到超临界CO2萃取物7个组分,超声波萃取物6个组分,室温冷浸法萃取物2个组分。将每个组分进行了质谱分析,结果表明,超临界CO2萃取的产物中大部分为甘草黄酮类物质、香豆精类物质及甘草次酸,而不含有分子量相对较大、极性较强的甘草酸。更多还原

【Abstract】 With the aim of extraction, separation and purification of medicine components from Liquorice, we performed extraction experiments of liquorice using various methods, including supercritical CO2 extraction, room-temperature immersion and ultrasonic extraction. The optimum extraction conditions were found, and the extracted products were analyzed by MS. The following results are obtained based on the experiments:Flavonoids were extracted from liquorice using supercritical CO2 extraction. A variety of factors were investigated, including liquorice granularity, extraction pressure, temperature, extraction time and flow rate of CO2. In addition, cosolvent type and its concentration and dosage were also examined. Based on the separate effect of these factors on the product yield, the optimal extraction conditions were determined. The product yield was 7.03% at 16MPa and 50°C.To obtain polar products from liquorice, we performed room-temperature immersion and ultrasonic extraction, and compared the three different extraction methods based on extraction efficiency and product distribution. The product yield was 7.72% and 8.92% with the ultrasonic extraction and the room-temperature immersion method, respectively. Besides, the product distribution was very different with the three different extraction methods. Following supercritical CO2 extraction, the material was subjected to ultrasonic extraction and an extraction yield of 4.85% was obtained. The total extraction yield from a combination of the two-extraction process was 11.88%, with flavonoids as the major product in supercritical CO2 extraction and Glycyrrhizic Acid in ultrasonic extraction.The crude extracts were separated by TLC and Column Layer Chromatography. It was found that SCCO2 extracts were composed of 7 group components, while ultrasonic extracts included 7 group components and room-temperature immersion extracts had 2 group components. The component identification of these groups were determined by MS. SCCO2 extracts had a lot of flavonoids, glycycoumarin and Glycyrrhetinic Acid. But Glycyrrhizic Acid, with high molecular weight and strong polarity, was very difficult to be extracted by SCCO2.更多还原