【作者】 宋春娜；

【导师】 徐永平；

【作者基本信息】 大连理工大学 ， 生物化工， 2008， 硕士

【摘要】 天然植物中含有丰富的活性物质,被广泛用于药品、保健品和化妆品中。我国拥有丰富的中药资源,但中药提取物的国际市场占有率还不足5%。目前,我国中药有效成分提取常采用传统的有机溶剂提取以及现代的提取方法,如超声波、微波、超临界和超微粉碎辅助提取。但这些提取方法存在有机溶剂使用量大,常具有毒性且易燃易爆,提取率低以及操作步骤冗杂。因此,如何实现药材的高效利用,开发绿色环保、低成本、技术成熟度高的提取技术无疑是一个亟待解决的问题。本研究采用微切助互作技术,以水作溶剂提取穿心莲内酯、松针总三萜酸以及刺五加中紫丁香苷。首先,筛选和确定了微切助互作技术辅助提取的最佳助剂;其次,初步考察目标提取物与助剂间的作用情况并比较不同预处理方法对各药材形态及提取率的影响;最后,在单因素试验基础上,通过正交试验优化提取工艺并与热回流提取比较。结果表明,经固态研磨后,穿心莲内酯可能与最佳助剂Na₂CO₃反应成盐,与羟丙基-β-环糊精（HP-β-CD）形成复合物;松针总三萜酸可能与最佳助剂Na₂CO₃反应成盐;刺五加中紫丁香苷与HP-β-CD形成复合物;以水作溶剂,微切助互作技术法的提取率显著高于物理混合及超微粉碎辅助提取;物料的粒度及扫描电镜分析表明经微切助互作技术处理后各药材的大部分细胞可能被充分破碎。微切助互作技术辅助提取穿心莲内酯的最佳工艺为:（1）碱作助剂。Na₂CO₃用量3%（w/w）,研磨时间45min(即物料粒度D₉₅≤37μm),水作溶剂,料液比为1:60 g:ml。（2） HP-β-CD作助剂。用水提取,HP-β-CD用量13%（w/w）,循环水温度70℃,研磨时间25 min。微切助互作技术辅助提取松针中总三萜酸的最佳工艺为:Na₂CO₃用量为5%（W/W）,研磨时间35min(即物料粒度D₉₅≤37μm),乙醇浓度为20%（v/v）,料液比为1:40 g:ml。以水替换乙醇,其提取率与20%（v/v）乙醇相当,提示可用水提取。微切助互作技术辅助提取刺五加中紫丁香苷的最佳工艺为:HP-β-CD用量为23%（w/w）,循环水温度40℃,研磨时间45min(即物料粒度D₉₅≤37μm)。与热回流提取比较,微切助互作技术辅助提取将物理法和化学法结合,以水作溶剂,具有提取率高,工艺简单,耗时短,绿色环保等特点,为穿心莲内酯、松针总三萜酸以及刺五加中紫丁香苷的提取提供了新途径。更多还原

【Abstract】 Natural plant contains a diverse group of bioactive substances with a broad range of applications in medicine, healthcare product and cosmetic. China is rich in medical herb resources, but has a weak market share （less than 5%） for plant extract in the world market. Past methods for extracting these bioactive compounds from complex plant matrixes have varied from traditional solvent extractions to more modern techniques such as supercritical fluid extractions, pressurized fluids extraction, microwave-assisted extraction, and ultrasound-assisted extraction. But there are many limitations of the present extraction technology: usage of organic solvents, often toxic and high flammable, low yields of an extraction for one stage of processing, as a corollary one multiple repetition of the extraction. The utilization of great quantities of organic solvents makes the technology very expensive, fire hazard and ecologically dangerous. Therefore, environmental friendly and industry-ready technique with low cost and enhanced efficiency is required in order to accelerate the development of herb extract industry in China.The present study was focused on the pressure-shear induced chemical transitions（PICT） assisted extraction of andrographolide from Andrographis paniculata, total triterpene acid from fir needles and syringin Eleutherococcus senticosus with water as solvent. First, the chemical reagent was selected according to the yield of target compounds by PICT assisted extraction; Second, a preliminary investigation was conducted on the interaction of the target compound-chemical reagent. Different pretreatment was compared with respect to their effects on the plant material morphology as well as the target compound yield. Finally, the PICT process was optimized based on both orthogonal and one-factor experiment, and was compared with conventional heat reflux extraction.Preliminary investigation showed that andrographolide could possibly be neutralized by Na₂CO₃, and certain complexes may have been formed between andrographolide and hydroxypropyl-β-cyclodextrin （HP-β-CD） after the solid grinding process; total triterpene acid could possibly be neutralized by Na₂CO₃; certain complexes may have been formed between syringin and HP-β-CD after the solid grinding process. The yield of PICT treated samples （extracting with water） was significantly improved （P <0.05） comparing with physical mixing and superfine grinding samples. Both particle analysis and scanning electron micrographs suggested that the plant cell wall could be broken up after the mechanochemcal treatment.The optimum parameters for PICT assisted extraction of andrographolide were as follows: （1） alkali reagent. Na₂CO₃ content, 3% （w/w）; milling period, 45min (particle size, D₉₅≤37μm); extraction solvent, water; liquid/solid ratio, 1:60 g:ml. （2） HP-β-CD reagent. HP-β-CD content, 13% （w/w）; circulating water temperature, 70℃; milling period, 25 min.The optimum parameters for PICT assisted extraction of total triterpene acid were as follows: Na₂CO₃ content, 5% （w/w）; milling period, 35 min (particle size, D₉₅≤37μm); extraction solvent, 20% v/v aqueous ethanol; liquid/solid ratio, 1:40 g:ml. Aqueous ethanol was replaced by water, and no significant difference in yield was observed with other optimized parameters settings.The optimum parameters for PICT assisted extraction of syringin were as follows: HP-β-CD reagent. HP-β-CD content, 23% （w/w）; circulating water temperature, 40℃; milling period, 45 min.Under the optimized parameters determined herein, significant enhancement such as improved yield, shorter time and more simplified procedures over heat-reflux extraction was observed, which makes PICT （a combination of physical and chemical method） a potential convenient tool for andrographolide from Andrographis paniculata, total triterpene acid from fir needles and syringin Eleutherococcus senticosus. Moreover, the favorable solvent is water, making PICT assisted extraction a less expensive and eco-friendly technique.更多还原