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Investigation On The Preparation, Recognition Behavior And Solid Phase Extraction Of Several Pharmaceutical Active Molecules Imprinted Polymers

Posted on:2016-05-26Degree:MasterType:Thesis
Country:ChinaCandidate:M M XuFull Text:PDF
GTID:2271330473450144Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
In present work, some small active drug molecules,like puerarin, vanillic acid, aubucin, rifamycin S; were used as templates molecules for the preparation of molecularly imprinted polymers by using different techniques including precipitation polymerization, surface imprinting polymerization and bulk polymerization, and so on. All of polymers were characterized by using SEM and FTIR. Also, we tested surface structure characters, dynamic adsorption, static adsorption, liquid chromatography of molecularly imprinted polymer by different ways. Adsorption isotherm and adsorption dynamics of molecularly imprinted polymers were obtained. Some of molecularly imprinted polymer were used as solid phase extraction media for the enrichment and separation of target compounds from crude extract of plant material, indicating a good applicability.Puerarin imprinted polymers microspheres(MIPM) were prepared by precipitation polymerization technique using puerarin as the template, MAA and EGDMA as functional monomer and cross-linker, respectively. Scanning electron microscope(SEM) was used for evaluating the morphology of polymer and static method for characterizing the adsorption behavior. Also, adsorption, desorption and solid phase extraction application for the MIPM in crude extraction solution of pueraria root was explored. Results indicated that the adsorption capacity for the optimized MIPM(MIP3) toward pure template reached 37.9mg/g, with a adsorption percentage of 96.3±1.81% toward target compound in crude extract solution. The desorption percentage varied within 27-34% when using water, methanol-acetic acid mixed solvent(9:1, v/v) and 50% methanol water solution as eluents, respectively, furthermore, the product desorped from the MIP3 using water as eluent possessed the highest content of puerarin(37.4±2.87%). 75% purity of puerarin product can be obtained by MIP3 single step solid phase extraction, with a puerarin recovery of 98.5%.A vanillic acid imprinted mesoporous silica polymers(MIPs) was prepared by copolymerizating a modified mesoporous silica molecular sieve with template molecule, functional monomer and cross-linker in present work. Interaction between the template and functional monomer was investigated by ultraviolet/visible spectrophotometry. This MIPs was characterized by Fourier transmission infrared spectrometry(FTIR) and scanning electron microscopy(SEM). Adsorption dynamics and thermodynamic behavior of the MIPs was explored and the selective recognition capability evaluated. Also, the applicability for this MIPs as solid phase extraction media was tested. Results indicated the 1:1(mole ratio) complex of vanillic acid-4-vinylpyridine might predominate in the pre-polymerization mixture and the MIPs obtained possessed rapid binding dynamics and higher affinity toward the template molecules, reaching adsorption equilibrium within 230 min with the highest adsorption amount of 50.7 mg/g. Freundlich model was shown best to describe isotherm.Aubucin imprinted polymers was prepared by bluk polymerization technique using Aubu cin as the template, 4-VP as functional monomer and EGDMA as cross-linker, which investigated the Interaction between the functional monomer-Co2+ and template-Co2+ by ultraviolet/is ible spectrophotometry. Molecularly imprinted polymer was characterized by Fourier transmi ssion infrared spectroscopy(FTIR) and Scanning electron microscope(SEM), which investig ated the static adsorption of molecularly imprinted polymer, and evaluated the selective recog nition of MIPs. By doing the chromatographic analysis, the mobile phase of separating these t hree similar compounds was optimized. the maximum absorption capacity is 84.6 mg/g. when the mobile phase is methanol-water(70%-30%,v/v), the best separation conditions of the three kinds of compounds is that the retention time of Aucubin is 5.742 min, the retention tim e of geniposide is 2.813 min, the retention time of pinoresinol is 2.647 min. So it is easy to dist inguish Aucubin from other two compounds.An anlogue of the compound 625, Rifamycin S, was used as the template for the preparation of molecularly imprinted polymers by bluk polymerization technique using MAA and EGDMA as functional monomer and cross-linker, respectively. The molecularly imprinted polymer were characterized by Fourier transmission infrared spectroscopy(FTIR) a nd scanning electron microscope(SEM). The static adsorption and dynamic adsorption experi ments was carried out and the results showed a rapid adsoprtion dynamics. Also, the maximum adsorption amount for the molecularly imprinted polymer toward the template and the compound625 was 25.45 and 19.86 mg/g. In addition, when using the MIP for the solid phase extraction of the target compound 625 from real crude extract, a recovery of 94.3 can be reached and higher purity of target compound can be obtained by the MIP solid phase extraction.
Keywords/Search Tags:Molecularly imprinted polymer, Aubucin, puerarin, Vanillic acid, RifmicinS
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