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The Synthesis And Application Research Of Organic And Hybrid Molecularly Imprinted Solid-phase Microextraction Medium

Posted on:2013-04-04Degree:MasterType:Thesis
Country:ChinaCandidate:C MaFull Text:PDF
GTID:2251330395986421Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Molecular imprinting polymers have many advantages,including strong ability to remove the matrix in the many stromas, materials’interior has porous structure, high mass transfer rate, and so on. So, molecular imprinting polymers are often used for solid phase microextraction(SPME). Combining with SPME, the meterials have a high selectivity ability in complex stromas to enrich the traces of analytet, and high selectivity, sensitive can be developed in this method. In this paper, two kinds of molecular imprinting polymers were prepared by molecular imprinting technique and they were used in SPME procedure. High selectivity, sensitive and rapid analytical methods for the determination of some environmental pollutants environmental samples and pesticide residues in food were developed. The main content of this paper is as follows:(1)The coating for stir bar sorptive extraction of caffeine were prepared by situ polymerization technique and its structure and characteristics were evaluated. And then it were applied for the selective extraction of caffeine in drinks simples. A rapid and sensitive method for the determination of caffeine in drinks simples using coating for stir bar sorptive extraction based on the molecularly imprinted polymer (MIP) combined with high-performance liquid chromatography (HPLC) was developed. By optimizing the polymerization conditions, such as the nature and amount of porogenic solvent and functional monomer, the molar ratio of the monomer and cross-linker, the time of prepolymerization process,the times of coating procedure,this materials was synthesized on the surface of a glass tube. The imprinted coating for stir bar sorptive extraction showed excellent affinity and highly specific recognition for the template caffeine and another two analogues,reached,the imprinted factors (IF) were4.42,4.39and4.19,respectively. The parameters such as the type of loading solution and eluent, and time of extraction and elution, the agitation speed were investigated and optimized. Under the optimum conditions, the method which has good stability and high precision (RSD<7.9%) was applied for the selective extraction of caffeine in three kinds of drinks.The linear range was5μg/L--150μg/L and the correlation coefficient of above0.997. The limits of detections (LODs) of caffeine was calculated to be1.86μg/L in drinks samples, The proposed method was successfully applied for the selective extraction and determination of caffeines in drinks samples.(2) Organic-Inorganic hybrid MIP monolith (OHMIP) for recognition isoprocarb were prepared by in routine sol-gel technique and situ polymerization technique and its structure and characteristics were evaluated. Then it were applied for the selective extraction of isoprocarb in rice simples. A rapid and sensitive method for the determination of isoprocarb in rice simples was developed. Various factors should be considered to obtain higher specific recognition ability and extraction efficiency for the target analyte, including the amount of porogenic solvent and y-MAPS,type of inorganic precursor, the molar ratios of inorganic alcoholysate and organic part,and so on. A isoprocarb OHMIP monolith was synthesized in a300μL of micro pipette tip. Comparing with non-imprinted (NIP) hybrid monolith,_the imprinted factors (IF) reached4.41. The MIP micro monolith were investigated through scanning electron microscopy, infrared spectrum and HPLC. The monolith was applied for the selective extraction of isoprocarb in rice simples. Several parameters were investigated, including the he type, flow rate and volume of eluent, flow rate and volume of sample solution, the type washing solution. Under the optimum conditions, the method has strong ability to remove the matrix in the many stromas, good stability and high precision, which satisfied the request of quantitative analysis.(3) Organic-Inorganic hybrid MIP monolith (OHMIP) for recognition carbaryl and naproxen were prepared by using of combinations of two template and its structure and characteristics were evaluated. On the basis of previous work, a rapid and sensitive method for the determination of carbaryl and naproxen was developed by optimizing part of synthesis conditions. The MIP micro monolith were investigated through scanning electron microscopy, infrared spectrum and HPLC. And was applied for the selective extraction of carbaryl and naproxen in complex real samples by investigating several parameters of solid phase microextraction. Under the optimum conditions, the method has strong ability to remove the matrix in the many stromas, good stability and high precision, which satisfied the request of quantitative analysis.
Keywords/Search Tags:Organic-Inorganic hybrid MIP monolith, coating for stir bar sorptive extraction, Double template, solid phase microextraction, caffeine, isoprocarb, carbaryl, naproxen
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