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Imprinted monolithic column and solvent extraction for chiral separation

Author: YangWeiJie
Tutor: ChenXiaoQing
School: Central South University
Course: Analytical Chemistry
Keywords: Molecularly Imprinted Monolithic column HPLC RAFT Polymerization Chiral extraction
CLC: O658.2
Type: Master's thesis
Year: 2010
Downloads: 166
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Abstract


This thesis is imprinted monolithic column and solvent extraction technology of chiral dibenzoyl tartaric acid and racemic ofloxacin chiral separation. (1) to dibenzoyl-D-tartaric acid (D-DBTA) template molecules, acrylamide (AM) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as crosslinking agent, a low-polarity toluene and dodecanol porogen is mixed in situ molecular imprinting technology, D-DBTA molecular imprinted monolithic polymer synthesis. On the basis to optimize the preparation conditions and the chromatographic conditions, DBTA racemate can be achieved within 25 min basic blot monolithic column chiral separation, separation of 1.25. In contrast, non-imprinted monolithic column DBTA racemate without any separation. Thermodynamic Study chromatography showed the presence of two different thermodynamic process in the temperature range investigated, the separation, and both meet the van't Hoff equation. Both thermodynamic process at the transition temperature, up to a maximum separation factor α. Scathcard analysis showed that only Imprinted polymers there exists a class of specific binding sites, and the dissociation constant and the maximum amount of apparent binding were: Kd = 5.457 x 10-4 mol / L, the Q max = 229.6μmol / g. Nitrogen specific surface adsorption experiments showed that a specific surface area of ??the imprinted polymer to 105m2 / g. The scanning electron microscopy (SEM) that has a large circulation channels imprinted monolithic column. When the flow rate of 1.2 mL / min acetonitrile as mobile phase, the column pressure is only 1.2 Mpa. (2) D-DBTA as template molecule, AM as the functional monomer, EGDMA as the crosslinker, dibenzyl trithiocarbonate (DBTTC) as chain transfer agent, the low polarity of the toluene and dodecanol as mixed porogen using reversible addition - fragmentation chain transfer (RAFT) polymerization situ preparation of D-DBTA molecular imprinted monolithic column compared legally prepared with traditional radical polymerization D-DBTA molecular imprinted monolithic column differences The results show that: the RAFT polymerization, the preparation of D-DBTA imprinted monolithic column pore size distribution is more uniform, and shows a higher binding properties of D-DBTA molecules. For chromatographic chiral separation DBTA racemate, which can effectively reduce the path effect, improve the chromatography column efficiency, shorten the time of chiral separation. (3) to two (2 - ethyl hexyl) phosphoric acid (D2EPHA) with tartaric acid derivative L-DBTA and methyl-dibenzoyl-L-tartaric acid (L-DTTA) as the mixed composite chiral selector, research ofloxacin (OFLX) enantiomer in n-octanol and water phases extraction distribution behavior. The effects of L-DBTA and L-DTTA, OFLX initial concentration, the molar concentration ratio of the impact of the extraction temperature chiral separation performance was extracted. The results showed that: When D2EPHA = 0.3 mol / L of L-DTTA: L-DBTA = 3:2, i.e. DTTA = 0.18 mol / L, DBTA = 0.12 mol / L, ofloxacin initial concentration of 0.2 mg / mL, extraction temperature 25 ℃, better extraction split the enantioselective β up to 2.43 D-and L-enantiomers of the partition coefficient of 10.20 and 4.20, respectively.

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CLC: > Mathematical sciences and chemical > Chemistry > Analytical Chemistry > Separation of elements and compounds > Extraction method
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