Font Size: a A A

The Study On Separation Of Aloe Bioactive Components And Chiral Compounds Base On Temperature Induced Aqueous Two Phase Extraction System

Posted on:2012-06-18Degree:DoctorType:Dissertation
Country:ChinaCandidate:J M XingFull Text:PDF
GTID:1484303353990129Subject:Applied Chemistry
Abstract/Summary:PDF Full Text Request
Separation of aloe bioactive components and chiral compounds was studied based on tritonX-114 temperature-induced aqueous two phase system.Firstly, the partitioning behavior of aloe polysaccharides and protein was studied in the aqueous two phase system. The factors affecting the recovery ratio were analyzed, namely the concentration of tritonX-114, pH, temperature and so on. Aloe polysaccharides and protein were purified, and the optimal separation condition were obtained, as follow the concentration of tritonX-114 was 4%, pH was 3, temperature was 50℃, the concentration of NaCl was 0.3 mol/L. The aloe polysaccharides were obtained under the optimal conditions, and their structure were investigated by IR and UV. The anti-oxidative activity of the·OH and O2-of aloe polysaccharides was discussed. The results showed that the aloe polysaccharides cound remove-OH and O2-.Secondly, the partitioning behavior of aloe-emodin was investigated. The factors affecting the recovery ratio were analyzed, namely the concentration of tritonX-114, pH and temperature.The optimal separation condition were obtained, the concentration of tritonX-114 was 10%, pH was 3, temperature was 40℃,the concentration of NaCl was 0.2mol/L Then poly(NIPAAM-co-AA)/EAA-β-CD was prepared by means of solution polycondensation, simultaneity was investigated by IR and NMR. The poly(NIPAAM-co-AA)/EAA-(3-CD was added in order to separate the aloeemodin. Several influence factors were investigated, such as concentration of poly(NIPAAM-co-AA)/EAA-β-CD, pH and adsorption time. The results showed that the recovery ratio of aloe emodin increased with the increasing poly(NIPAAM-co-AA)/EAA-β-CD concentration and the adsorption time. The pH had large influence on adsorption of aloe emodin, the recovery ratio increased remarkably before pH was up to 7, and the recovery ratio reached maximum at pH 7. Thirdly, the partitioning behavior of mandelic acid was studied on the isopropyl alcohol/salt and tritonX-114 temperature induced system. The results showed that the mandelic acid tended to be existed in the isopropyl alcohol phase, and while in the aqueous phase in the tritonX-114 temperature induced system, so the tritonX-114 temperature induced system was used as chiral recognition system. The chiral recognition of mandelic acid was investigated in the tritonX-114//n-amyl-L-tartrate/teasaponin and tritonX-114/(3-CD system. Several factors were studied such as content of teasaponin, temperature and so on. The results showed that the tritonX-114/ n-amyl-L-tartrate /teasaponin system was better than the tritonX-114/(3-CD system. The separation factor increased with the increasing of teasaponin concentration and temperature, and the optimal chiral recognition conditions of aqueous two phase system was obtained, the concentration of teasaponin was the 0.51mmol, the n-amyl-L-tartrate was 1.4mmol, temperature 55℃.The largest separation factor was 1.29.Fourthly, the copper (Ⅱ) formed a 2:1 complex withβ-CD in an alkaline solution,which was isolated from solutions by addition of ethanol. The complex of structure was characterized by IR, UV and XRD. The chiral recognition system was established by adding Cu2-β-CD in the tritonX-114 aqueous two phase extraction system, which preferentially recognize the (R)-enantiomer and (S)-enantiomer, respectively. Factors affecting the extraction mechanism are analyzed, namely the concentration of Cu2-β-CD and tritonX-114, the types of salts, pH, and temperature. It was found that the concentration of Cu2-β-CD and temperature were the most important influence factors for chiral separation of mandedlic acid. The experimental results showed that the separation factors increase with pH and concentration of tritionX-114, and the maximum separation factors was 5.05. The addition of inorganic salt had large influence on separation factor, and it decreases when the salt is added in the aqueous two phase extraction system.Fithly, the chiral recognition system was established by adding HP-β-CD and ionic liquid into the tritonX-114 aqueous two phase extraction system, which preferentially recognize the (R)-enantiomer and (S)-enantiomer, respectively. The result showed that inclusion compound of tritonX-114 with HP-β-CD andβ-cyclodextrin derivatives was destroyed. So the separation factor inceased with the increase of ionic liquid concentration, and the separation factor reached maximum at the concentration 0.3mmol/L. It also was found that the temperature and pH were important influence factors for chiral separation of mandedlic acid. The separation factor decreased with increasing of temperature and pH.Finally, inclusion complex was obtained by grinding method. The inclusion complex formation of mandedlic acid with HP-β-CD was studied by IR and DSC. The inclusion behavior between HP-β-CD and R,S-mandedlic acid was studied by UV spectrophotometry, respectively. The results indicate that UV absorbance decreased with the increase of HP-β-CD concentration. R, S-stability constants were 140 and 103 by using Hildebrand-Benes.T, respectively. The separation factor was 1.36.
Keywords/Search Tags:temperature induced, ionic liquid, chiral recognition, inclusion complex
PDF Full Text Request
Related items