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Preparation And Investigation Of MIPs/DMIPs For Separating And Enriching Trace TBPPA In Environmental Water Samples

Posted on:2014-04-10Degree:MasterType:Thesis
Country:ChinaCandidate:W ShenFull Text:PDF
GTID:2251330398993301Subject:Drug analysis
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Tetrabromobisphenol A (TBBPA) is potential one of persistent organic pollutants with seriously toxicological effects. In the past several years, TBBPA has been excessively used in electronic equipments, textiles and plastics. It can release to environment and finally accumulate in human body, which is harmful to human health. The accurate and specific determination of TBBPA in complex matrices can provide reference and supports for risk assessment and migration study of TBBPA.In this study, molecularly imprinted polymers (MIPs) and dummy molecularly imprinted polymers (DMIPs) for TBBPA were prepared on the surface of silica particles with a sol-gel process and the MIPs/DMIPs were applied to the purification, separation and enrichment of trace TBBPA in environmental water samples.MIPs have attracted more and more attention because of their predetermination, specific recognition and practicability for analytes. In the study, by adopting TBBPA as the template,(3-Aminopropyl) triethoxysilane as the functional monomer, ethyl silicate as the cross-linker, TBBPA imprinted polymers were prepared with a sol-gel process on the surface of silica nanoparticles. Fourier transform infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM) were performed to ascertain the interaction of MIPs. The MIPs were uniformly dispersive with narrow size distribution. The toluene was chosen as the adsorption solution. Static adsorption text, dynamic adsorption text and competitive adsorption text were conducted respectively to evaluate the MIPs. The maximum adsorption capacity of the MIPs for TBBPA was approximately183μmol/g (61.90mg/g), which was about3.2times as much as57μmol/g of the non imprinted polymers (NIPs). The MIPs could reach adsorption equilibrium in20min which showed fast binding kinetics for TBBPA. Through competitive adsorption text, it was found the MIPs could selectively retain TBBPA from the mixture of TBBPA and its three structural analogous. In addition, the MIPs were applied to the purification of TBBPA contaminated water with a desirable result. However, there was a serious disadvantage of the MIPs that was the leakage of the templates. This would affect the quantification of trace target analytes in complex matrices.To avoid the leakage of target analytes, TCBPA, a structure analogous of target analyst is selected for preparation of imprinted polymers in the second part. In this study, DMIPs for TBBPA were prepared on the surface of micro-nano silica particles with a sol-gel process. TCBPA was chosen as the template. The DMIPs were applied to the determination of trace TBBPA in environmental water samples. FT-IR and TEM were performed to ascertain the interaction of DMIPs. The DMIPs were uniformly dispersive with narrow size distribution. The toluene was chosen as the adsorption solution. Static adsorption text, dynamic adsorption text and competitive adsorption text were conducted respectively to evaluate the DMIPs. The maximum adsorption capacity of the DMIPs for TBBPA was approximately230μmol/g (77.28mg/g), which was about6times as much as40μmol/g of the NIPs. The DMIPs could reach adsorption equilibrium in20min which showed fast binding kinetics for TBBPA. Through competitive adsorption text, it was found the DMIPs could selectively retain TBBPA from the mixture of TBBPA and its three structural analogous. In addition, a method for the determination of trace TBBPA in environment water samples was established by the dummy molecularly imprinted solid phase extraction coupling with high performance liquid chromatography. Under the built method, the linear range of TBBPA standard aqueous solution was0.2-8.0ng/mL with a correlation coefficient of0.9947and the limit of detection was0.1 ng/mL. The recoveries of TBBPA at1.0ng/mL spiked with in water samples were in the range of91.1%-93.8%and the relative standard deviations were all less than9.0%(n=5). The results showed that the properties of the DMIPs were superior and could be used to separate and enrich trace amount of TBBPA in environment water samples.
Keywords/Search Tags:Molecularly imprinted polymers, Purification, Separation, Enrichment, Sol-gel, Tetrabromobisphenol A, Tetrachlomobisphenol A
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