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微波辅助浊点萃取法提取分离天然产物有效成分
Alternative TitleMicrowave-assisted Cloud Point Extraction and Separation of Active Ingredients from Natural Prod
邓福礼
Subtype博士
Thesis Advisor刘会洲
2013-05-01
Degree Grantor中国科学院研究生院
Degree Discipline化学工艺
Keyword微波辅助浊点萃取   非离子表面活性剂   罗汉果甙v   辣椒碱   二氢辣椒碱
Abstract浊点萃取是一种基于胶团增溶和热至分相的分离技术,经过简单操作便可实现溶质的富集与分离,并且能够获得较高的萃取率与富集率。微波辅助萃取是将微波加热和溶剂萃取相结合,与传统的提取方法相比,微波辅助萃取提取天然产物活性成分具有提取时间短,溶剂用量少,提取率高等优点。本文研究了天然抗氧化剂在非离子型胶团中的增溶规律以及非离子型表面活性剂水溶液的分相行为,并结合微波辅助萃取与浊点萃取研究了提取富集天然产物有效成分的方法和工艺。 利用核磁和光散射技术研究了抗氧化剂在非离子型表面活性剂胶团中的增溶规律。罗汉果甙V使非离子型表面活性剂TritonX-100(TX-100)和Genapol X-080(GX-080)水溶液的浊点温度升高,胶团水力学半径和聚集数减小。而没食子酸、没食子酸甲酯和没食子酸丙酯使TX-100和GX-080的浊点温度降低,胶团半径和聚集数增大。其中没食子酸丙酯的影响最大,没食子酸甲酯次之,没食子酸最小。NOESY实验发现没食子酸丙酯的甲基和苯环与TX-100的 EO链段有弱的相互作用;没食子酸丙酯的苯环与GX-080的EO链段存在相互作用,且丙酯的甲基与GX-080的甲基有较强的相互作用。表明没食子酸丙酯增溶在TX-100 的EO链段形成的胶团壳层;而没食子酸丙酯的甲基进入了GX-080胶团的内核同时苯环与GX-080的EO链段有相互作用,增溶在胶团的“栅栏”中。通过对不同条件下丙酯的表观扩散系数进行拟合,得到了丙酯与非离子型表面活性剂之间的结合常数,其值分别为700 ± 65 M-1(GX-080)和352 ± 30 M-1(TX-100)。 考察了非离子型表面活性剂的浊点分相行为,并应用TX-100和GX-080成功地从模拟体系中富集亲水性的罗汉果甙V。表面活性剂的浓度增加,罗汉果甙V的浊点萃取率增加,同时凝聚相体积分数增加。而罗汉果甙的浓度在试验范围内对萃取率的影响较小。未加盐时,温度对分配系数影响较小,温度升高引起凝聚相体积分数减少是浊点萃取率降低的主要原因。无机盐氯化钠的加入使亲水性的罗汉果甙V萃取率显著增大,凝聚相体积分数减少,富集因子增加,分配系数显著增大。 应用微波辅助浊点萃取法提取富集与分析罗汉果中的主要有效成分罗汉果甙V。与水,乙醇及甲醇等溶剂比较,加入非离子表面活性剂TX-100和GX-080都提高了罗汉果甙V的提取率。以5% GX-080为提取溶剂,罗汉果甙V的一次提取率达到96.8%。在浊点萃取时,盐析型无机盐的加入降低了浊点,提高了罗汉果甙V的分配系数,使浊点萃取率增加。当加入0.25g/ml的氯化钠,在50 oC时平衡30 min,萃取率达到80.7%,富集因子达10.8。 采用微波辅助浊点萃取法从干辣椒中提取分离疏水性有效成分辣椒碱和二氢辣椒碱。以5% TX-100水溶液为提取溶剂,胶团的增溶作用使辣椒碱和二氢辣椒碱的提取率比以水为溶剂提高了约5倍,与甲醇和乙醇的提取效果相当。与索式提取法相比,微波辅助胶团萃取具有更高的提取效率。浊点富集过程中加入0.1 g/mL的氯化钠,当萃取温度为70 °C,平衡时间为10 min,辣椒碱和二氢辣椒碱的浊点萃取率分别为97.8±2.5%和96.8±1%,富集因子达到12以上。 微波辅助浊点萃取法是一种绿色、快速、有效地提取富集天然产物有效成分的方法。
Other AbstractCloud point extraction (CPE) based on micellar solubilization and unique phase separation behavior can be used for extraction and preconcentration solute with high extraction recovery through a simple operation. CPE is an environmentally friendly technology, which has been extensively applied for extraction of compounds in various matrices. Microwave-assisted extraction (MAE) is a technique that combines microwave heating and traditional solvent extraction. MAE has many advantages, such as higher extraction yield, shorter extraction time and less solvent, over conventional method of extraction of active ingredients from natural products. In this dissertation, the solubilization of antioxidants in nonionic micelles as well as the phase behavior of aqueous nonionic surfantant solutions were investigated. MAE and CPE were applied for extraction and preconcentration of active ingredients from natural products. The solubilization of natural antioxidants in nonionic micelle was investigated by NMR and light scattering techniques. The cloud point (CP) of aqueous solutions of Triton X-100 (TX-100) and Genapol X-080 (GX-080) increased with the addition of mogroside V while the hydrodynamic radius as well as the aggregation number of nonionic micelles decreased. However, the CP of aqueous solutions of TX-100 and GX-080 decreased and the hydrodynamic radius as well as the aggregation number increased.in the presence of gallic acid (GA), methyl gallate (MG) and propyl gallate (PG). The depression of CP by antioxidants on the TX-100 and GX-080 systems was in the order PG>MG>GA. The chemical shifts of protons signals of antioxidants (GA, MG and PG) were shifted upfield. The nuclear Overhauser effect (NOE) experiments indicated that PG is solubilized in the shell region of TX-100 micelles, while in GX-080 micelles the aromatic protons of PG interact with the hydrophilic EO chain and more hydrophobic parts penetrate into the micelle core. The values of Ka for GX-100 and TX-080 binding to PG were found to be 700 ± 65 M-1 and 352 ± 30 M-1, respectively.
Pages115
Language中文
Document Type学位论文
Identifierhttp://ir.ipe.ac.cn/handle/122111/8244
Collection研究所(批量导入)
Recommended Citation
GB/T 7714
邓福礼. 微波辅助浊点萃取法提取分离天然产物有效成分[D]. 中国科学院研究生院,2013.
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