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Preparation Of Zidovudine And Nateglinide Imprinted Polymer And Application In Solid-Phase Extraction

Posted on:2012-08-22Degree:MasterType:Thesis
Country:ChinaCandidate:Y M SunFull Text:PDF
GTID:2214330338456681Subject:Drug analysis
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Molecular imprinting technique is a polymer synthesis technique which was designed and synthesized on the basis of the spatial structure and the properties of target molecules, so the resulting polymer molecules has the characteristics of the intended target,selectivity and the recognition. At present, the technology has been applied to organic chemistry, separation chemistry, analytical chemistry and other fields, especially the separation and analysis of drugs, the enrichment and purification of Chinese herbal medicine active ingredients, the testing of biological sensors, the environmental samples the clinical medical and so on.Zidovudine was the first drug that used for AIDS treatment; Nateglinide is a new novel of glucose regulator phenylalanine. In this thesis, Zidovudine was used as imprinted molecule, N, N-dimethyl formamide was used as pore-forming agent, a-methyl acrylic acid (MAA) was used as functional monomer, and the ethylene glycol dimethyl Acrylate (EDMA) was used as crosslinker, initiated by the initiator of azobisisobutyronitrile (AIBN) to engender a system of molecular imprinted polymer; Nateglinide was used as imprinted molecule, Chloroform was used as pore-forming agent, Acrylamide (AM) was used as functional monomer, and the ethylene glycol dimethyl Acrylate (EDMA) was used as crosslinker, initiated by the initiator of azobisisobutyronitrile (AIBN) to engender a system of molecular imprinted polymer. Meanwhile, a preliminary study and application of polymer was conducted. The main contents are shown as follows:1. In this case, Zidovudine and Nateglinide was used as imprinted molecule, the imprinted polymer of Zidovudine and Nateglinide was synthesized. The prepared MIP has excellent performance, through the optimization of the proportion of monomer, crosslinker and polymerization temperature factors. It was shown that the property of Zidovudine MIP were satisfactory when the ratio of template molecule, monomer and crosslinker was 1:4:20, and the property of Nateglinide MIP were satisfactory when the ratio of template molecule, monomer and crosslinker was 1:4:24, the polymerization temperature was 60℃2. Zidovudine and Nateglinide MIP evaluation:The composition and properties of imprinted polymers were analyzed by infrared spectroscopy, UV spectroscopy, statics adsorption, specific surface area comparison and selective test, the results show that molecular imprinted polymer was porosity, and specific identifiable.3. Establish Zidovudine MISPE method:The imprinted polymer of Zidovudine was used in solid-phase extraction, the using conditions of extraction column were optimized. MISPE extraction condition were optimized as:3 mL methanol, and 3 mL water were used to activate the MIP column respectively, loading with 3 mL water, washing with 1mL water and eluting with 3 mL 5% Acetic acid /methanol. Under these conditions different concentrations (0.3伍800μg/mL) of Zidovudine could be recovered. The recoveries were between 96.9% to 73.8%, Qmax is 42.4 mg/g. Solid-phase extraction coupled to HPLC for the efficient determination of AZT in Urine. The standard addition recoveries of 0.4,2 and 4μg/mL were 87.3%,93.4% and 94.5% respectively.4. Establish Nateglinide MISPE method:Nateglinide MISPE extraction condition were optimized as:3 mL methanol, and 3 mL water were used to activate the MIP column respectively, loading with 3 mL 30% methanol/water, washing with 1mL 20% methanol/water and eluting with 3 mL 5% Acetic acid/methanol. Under these conditions different concentrations (0.07-90μg/mL) of Nateglinide could be recovered. The recoveries were between 96.1% to 70.8%. Solid-phase extraction coupled to HPLC for the efficient determination of Nateglinide in Plasma. The standard addition recoveries of 0.05,2 and 4μg/mL were 74.9%,89.6% and 92.2% respectively.
Keywords/Search Tags:Zidovudine, Nateglinide, Molecular imprinting, solid-phase extraction
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