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Solid-phase Extraction Based On Magnetic Nanoparticles For The Determination Of Microcystin-LR In Water Samples Coupled With High Performance Liquid Chromatography

Posted on:2016-01-07Degree:MasterType:Thesis
Country:ChinaCandidate:H SunFull Text:PDF
GTID:2181330467499998Subject:Analytical Chemistry
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Sample preparation is a top priority throughout the analysis process, magneticsolid-phase extraction (MSPE) with magnetic or magnetizable material and developed anovel solid-phase extraction analysis techniques. MSPE technology is a preconcentrationand separation of sample pretreatment method, which can quickly analyze and deal with alarge volume of environmental samples, high enrichment efficiency, less timeconsumption, superiority of preconcentration with environmentally harmful substances.MSPE is a widely used method for preconcentration and separation of trace target analytebecause of its special advantages such as simple, less organic solvents consumption, easymagnetic separation, automation. Using magnetic solid phase extraction material forpreconcentration and separation of sample, solve the presence of traditional sorbent thesolid-liquid separation difficult problems. Owing to its outstanding features and potentialapplications, MSPE technology give rise to analysis workers widespread attention in recentyears.Magnetic nanoparticles have unique magnetic properties and excellent physical andchemical properties, due to strong coordination ability of metal or metal oxide on itssurface, it can be easy to carry out the function of the modification. the modified magneticnanoparticles has been given new properties, such as a larger surface area, strong chemicalstability, biocompatibility and specificity of high adsorption performance. the exploitationof various magnetic solid phase adsorbents and the development of MSPE technologyinevitably release distinctive radiance in environmental, biomedical, food applications.We synthesized two novel magnetic material as solid phase extraction adsorbent,preconcentration and separation of biological contaminants in the water-microcystin(MC-LR), around its adsorption properties expand the following contents:(1) firstly, synthesized spherical Fe3O4magnetic nanoparticles by hydrothermal method, using St ber method coats SiO2/CTAB shell, then remove the CTAB formmesoporous, finally, Cu2+functionalization modified on its surface, obtain mesoporousFe3O4@SiO2@Cu2+magnetic microspheres. Applying it as a solid phase extractionsorbents, combining high-performance liquid chromatography establish a MSPE-HPLCanalysis method with separation and preconcentration of MC-LR. the extraction anddetection conditions have been optimized in detail.Various experimental parametersincluding the linear range, precision, limit of detection, limit of quantitation to verify theanalysis method, the method for MC-LR extraction recoveries of81%.(2) Via one step of hydrothermal synthesis, We prepare CuFe2O4magneticnanoparticles, the magnetic materials were used as the extraction agent, the development ofa separation and detection of MC-LR MSPE-HPLC method. magnetic nanoparticles werecharacterized, Various experimental parameters affecting the extraction recovery ofMC-LR were investigated and optimized including adsorbent dosage, extraction time,sample pH, the type of eluent, desorption of time and volume.The limit of detection forMC-LR is0.021μg/L in this analysis method.In summary, magnetic nano-materials were prepared through the new synthesismethods and the products were successfully applied to remove pollutants from water. Thisapproach provided a simple and economical method for preparation of multifunctionaladsorbents possessing well magnetic responsibility and dispersibility in solvents. Theadsorbents were also evaluated to bear excellent adsorptivity for biological contaminant(MC-LR). Although the techniques still have not been widely applied in water treatmentsystems, the functionnal magnetic adsorbents were recommended for potential applicationsto remove biological contaminants from polluted water.
Keywords/Search Tags:Magnetic nanoparticles, solid-phase extraction, microcystins, separate, enrichment
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