Preparation of novel functional materials and pollutants in the environment chromatographic detection

　　Title: Preparation of novel functional materials and pollutants in the environment chromatographic detection
　　Author: Ji Yongsheng
　　Degree-granting units: Lanzhou University
　　Keywords: Solid phase extraction;; functional materials;; high-performance liquid chromatography;; environmental pollutants
　　Abstract:
　　With the development of society, industry, agriculture and human life have given environment pollution, these pollutants in air, water, soil or plants and animals, directly or indirectly cause harm to human health. In the study of environmental pollution problems, is bound to exist in a variety of environmental pollutants analysis and detection, must be the establishment Rare earth magnets of environmental pollutants analysis, chromatography is the most widely used analytical methods. Because the presence of pollutants is more complex media usually takes a certain degree of separation and enrichment of pollutants sample processing before analysis. SPE is widely used in sample preparation area, preparation of adsorption, selective adsorption material is a good key to solid-phase extraction. This paper complex environmental samples for the detection of organic pesticides and estrogens were prepared by several functional materials, material properties were characterized, and its stationary phase for the solid-phase extraction in environmental samples to establish a method of analysis of target pollutants , mainly for the following aspects of innovative research.
　　1 to C18 as the stationary phase film produced a stirring rod solid-phase extraction, enrichment of the water used for pesticide MET optimize the extraction conditions for the establishment of the Yellow River water MET detection methods.
　　(2) prepared by oxidation of carbon nanotubes as the stationary phase of SPME fiber, carbon nanotubes studied from the water-rich oxide carbendazim, thiabendazole and thiophanate-methyl of the potential and the adsorption mechanism the study. Finally, the self-made SPME fiber and high-performance liquid chromatography combined with UV detection system set up analytical methods, and successfully applied to real samples of carbendazim, thiabendazole and thiophanate-methyl detection. Analysis of the actual sample recoveries 75.7-104.5%, linear range 5-500 ng mL-1, the square of the correlation coefficient 0.9978-0.9984, the detection limit 0.3-1.5 ng mL-1, precision relative standard deviation of 2.3- 10.5%.
　　3 Select the β-cyclodextrin as ligand synthesis of magnetic nano-materials as solid-phase extraction adsorbent, the nature of magnetic materials by infrared, transmission electron microscopy, to characterize the vibration magnetometer. The solid-phase extraction and magnetic separation technologies, bisphenol A (bisphenol A, BPA) and diethylstilbestrol (diethylstilbestrol, DES) for the target to study the synthesis of functionalized magnetic nano-materials as solid-phase extraction adsorbent potential. Optimize the impact of solid-phase extraction conditions such as sample volume, http://www.chinamagnets.biz/ sample pH, extraction time, desorption solvent. In a 250 mL sample, 0.1 g adsorbent, 3 mL of methanol containing 1% acetic acid elution conditions, all of the extraction operation in less than 25 min to complete. Finally, the solid-phase extraction and liquid chromatography combined with the establishment of tap water, river water, wastewater BPA and DES, the detection method. Analysis of samples spiked recovery of 80-105%, relative standard deviation of less than 7%, BPA and DES detection limits were 20.0 ng L-1, 23.0 ng L-1. Experimental results show that the established method of analysis of water samples for rapid analysis of trace.
　　4 to BPA as a template molecule, 2 - vinylpyridine as functional monomer, ethylene glycol dimethyl acrylate as crosslinker, the use of microemulsion polymerization of magnetic molecularly imprinted microspheres. By electron microscopy, vibrating magnetometer characterization of its morphology and magnetic properties. The separation of magnetic and magnetic combination of molecular imprinting establishment of environmental water samples and enrichment of BPA in milk by solid phase extraction method to optimize the adsorbent mass, sample pH, extraction time and other parameters, the optimal conditions in 15 min to complete solid phase extraction. The solid-phase extraction and liquid chromatography combined with the establishment of environmental water samples and testing of BPA in milk analysis. The method to achieve a large volume of samples fast and accurate analysis of BPA.
　　5 to C8 and polyethylene glycol for the synthesis of both ligand hydrophobic, hydrophilic and biocompatible magnetic nano-materials. The synthetic materials used were infrared, electron microscopy, elemental analysis of its morphology and composition. Vibration sample magnetometer to measure magnetic properties. Investigated by adsorption of its adsorption properties, and applied to serum sulfa enrichment.
　　6 semi-empirical quantum chemical PM3 method to calculate 130 descriptors of organic compounds, compounds with heuristics, respectively, in the whole of the three-dimensional gas chromatography column retention set up the corresponding quantitative structure - retention relationship model, and models have been tested. The model showed a good linear correlation coefficient squared greater than 0.88, the standard deviations were less than 0.105, leave-one cross-validation squared correlation coefficient with the model rather, that the model has good stability. Compounds showed that the model predicted a more accurate predictive capability.
　　Degree Year: 2010