| Organic polymer monolith column is a new type of miniaturized samplepretreatment strategy based on in-tube solid phase microextraction. As an extractionmedium, organic polymer monolith column has several advantages of goodbiocompatibility, high enrichment efficiency, simple preparation process, wide pHrange, and little sample consumption, etc. It combines concentration, extraction,separation, purification, moreover, it is rapid, sensitive, simple operation, and easy torealize automation. However, it also has some disadvantages, such as swelling inorganic solvent and decreasing mechanical stability, which may affect its life.Macrocyclic compounds have a variety of applications, such as molecularrecognition, supramolecular self-assembly, and bionic materials. In recent years,they have been applied in the enrichment of material and has developed very rapidly.Cyclodextrin and cucurbituril are representatives of macrocyclic compounds, both ofwhich have cavities and can easily form host guest compounds. Hydrogen bond,hydrophobic, and π-π interactions may exist between them and other compounds. Inaddition, they both have a variety of functional groups on the surface, which makesthem easily modified. In the present study, cyclodextrin and cucurbituril wereemployed for the modification of organic polymer monolithic column and used asenrichment materials. The novel monolithic material combines the advantages ofmacrocyclic compounds and polymers. The modified polymer monolithic columnswere coupled with gas chromatography and high performance liquid chromatography and applied to the determination of organic pollutant in food,environment, and biological source. The main points of this thesis are described asfollows:1. A poly(butyl methacrylate-co-ethyleneglyceldimethacrylate)(poly(BMA-EDMA)) monolithic column was prepared with an in situpolymerization method and modified with allylamine-β-cyclodextrin (ALA-β-CD)and nano-cuprous oxide (Cu2O). A polymer monolith microextraction method wasdeveloped with the modified monolithic column for the preconcentration ofpolychlorinated biphenyls combined with gas chromatography–electron capturedetector. Various parameters affecting the extraction efficiency were investigatedand optimized. Under the optimum experimental conditions, we obtained acceptablelinearities, low limits of detection, and good intra-day/inter-day relative standarddeviations. When applied to the determination of polychlorinated biphenyls in winesamples, low limits of detection (0.09ng/mL) were obtained under the preoptimizedconditions (sample volume1.0mL, sample flow rate0.1mL/min, eluent volume0.1mL, and eluent flow rate0.05mL/min). In addition, the present method wasemployed to determine polychlorinated biphenyls in red wine samples and theaccuracy was assessed through recovery experiments. The obtained recovery valueswere in the range of78.8–104.1%with relative standard deviations less than9.0%.2．Monolithic poly(glycidyl methacrylate-co-ethylene dimethacrylate) capillarycolumns incorporated with cucurbit[6]uril pseudorotaxane (CB[6]MR) wereprepared and used in polymer monolith microextraction (PMME) for the separationand preconcentration of nitroaromatics. The introduction of CB[6]MR to theglycidyl methacrylate-based monolith enhanced the column efficiency by24.5–35.5folds because of the hydrophobic interaction, electrostatic interaction, hydrogenbonds, and π-π interaction between CB[6]MR and nitroaromatics. An orthogonalexperiment design, L16(45), was applied to arrange and optimize the experimentalconditions. Under the optimum conditions, nitroaromatics were simultaneouslydetermined with good linearity and low limit of quantification (0.069–0.163ng/mLat a signal-to-noise ratio of10). The developed method was applied for the determination of nitroaromatics in water and blood samples, illustrating satisfactoryrecovery (83.2–107.9%and88.2–112.5%) and reproducibility (relative standard... |
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