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Study Of Synthesis & Characterization Of Chiral MOCPs And The Separation To Papain

Posted on:2008-12-23Degree:MasterType:Thesis
Country:ChinaCandidate:K ZhangFull Text:PDF
GTID:2144360215489775Subject:Medicinal chemistry
Abstract/Summary:PDF Full Text Request
Chirality is one of the essential characters for biology systems. Many biological macromolecules are chiral, like enzyme, carriers, acceptors, plasma proteis, and polysaccharide. Chiral medicines take a large proportion in all medicines. As reported, natural and semi-synthesized medicine almost has chirality, 40% synthesized medicine has chirality, and half of 700 medicines in common use have at least one chiral centre. Metal-Organic Coordination Polymers (MOCPs), which keep some properties of both organic macromolecules and inorganic metal compounds, are forming one kind of novel metal-organic hybride macromolecular materials with some novel structures and peculiar functions. For porous MOCPs their inner-hole sizes and shapes could be controlled by selecting metal ions and ligands, the so-called building blocks, and reaction conditions. Owing to MOCPs'predominant physical and chemical specialities, they have attractive potential in the areas as shape selective and chiral catalysis and separation, molecular identification, photoelectric technology, sensors, biological simulation, micro-reactors, clinical medicine, etc. If making appropriate choices in ligands, we could build the chiral space groups in holes, obtaining chiral MOCPs, which are promising in pharmaceutical separation.In this paper, using Cd (Ⅱ) as the center ion and iso-nicotinate as the ligand, we got the varied shapes and granularity MOCPs crystal with low temperature hydrothermal synthesis. Aimed at some factors that influnence crystal formation greatly, such as reactant ratio, reaction time, solvent, temperature and reaction container, we ran systematical experiments and conducted detailed analysis. Furthermore, we used element analyzer to determine the polymer's element proportion; characterized with IR spectra to affirm the organic groups in the frameworks; used single-crystal X-ray diffraction to determine the crystal structures and compositions of frameworks; utilized N2 adsorption isotherms at low temperature to mensurate the specific surface area and pore size distribution and scaled the thermal stability with TGA/DGA analysis. Moreover, we tested the solubility and fluorescence property. After above all, we prepared a chromatogram column with the chiral MOCPs and separated the papain. The separation effect was checked up by a G-250 method. Finally, we did some research about the influence of column separation on the enzyme catalyzed kinetics.In addition, we optimized some systhesis conditions, such as temperature, reactant ratio and dosage and found that polymer crystal could be hydrothermally synthezied from Cd2+ and iso-nicotinate ligand at lower temperature (less than 100℃). Compared with common hydrothermal synthesis, we enhanced the productivity by 10-30% and shorten the reaction period more than 50%. The MOCPs could be prepared conveniently and efficiently. The MOCP [(C12H16CdN2O8) n] belongs to triclinic crystal system without inter-penetration and crystallizes in a chiral space group. The MOCP has BET specific surface area up to 271.6m2g-1 and the everage pore diameter is 44.33?. The stable structure keeps until 420℃due to the existence of rigid benzene annulus. Besides, the polymer displays its chemical stabilization greatly when exposed in air. It also holds nicer anti-dissolved property towards varied common organic solvents and solutions in different pH values. Using the chiral MOCPs as the separation reagent, we separated the papain with a filled column. The results showed that the column has higher selectivity compared with silica gel column. The column separation efficiency is over 95%, much higher than that of the traditional silica gel column, from the measured enzyme concentration in the eluentfraction. According to the results obtained from the separating experiments on a group of small molecules, we proposed a possible separation mechanism. Furthermore, because of the function of Cd (Ⅱ) to the given groups in papain, we completed the separation and purification; it resulted in the improvement of enzyme specific activity and promoted the enzyme's hydrolyzation catalysis.
Keywords/Search Tags:Chiral, Metal-Organic Coordination Polymers, Hydrothermal Synthesis, Characterization, Chromatogram Column Separation
PDF Full Text Request
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