Study On A New Solid Phase Extraction Method Based On Metal - Organic Skeleton Material

With the development of industrial production and the modernization of the city, the environmental pollution is more and more serious. If water pollutants enter our body, the normal physiological metabolism will be impacted. PAEs have shown teratogenic, carcinogenic, reproductive and developmental effects. Plant growth regulators will be left in the water, causing some damage to the human body. UV absorbers from the cosmetics and industrial products will be in a variety of ways into the water, so the environment and human’s body will be harmed in a certain extent. Therefore, the establishment of rapid and sensitive methods for the determination of trace amounts of pollutants in environmental and biological samples is necessary. In order to obtain the accurate analysis results, choosing the appropriate sample preparation technology is commonly used before analyzing instrument separation and enriching of trace components. Solid phase extraction has many advantages, such as low organic solvent consumption, high recovery rate and high enrichment ratio, variety of material and so on. So it is used increasingly in the modern instrument detection technology, and the magnetic solid phase extraction method is more and more popular because of its easy operation. Generally, the solid phase extraction used adsorption material. In this work, metal-organic framework materials are chosed as the adsorbent. They have a broad application prospect in analytical chemistry, especially in environmental analysis, food analysis, and other fields because of its porous, large specific surface characteristics. This work uses solid phase extraction method to enrichment and separation of trace pollutants in the samples. The main works are as follow:Chapter One: We described the metal-organic framework materials and their application in solid phase extraction. And the recent developments of high performance liquid chromatography（HPLC） were introduced.Chapter Two: In our work, we developed a simple and facile synthetic strategy to prepare Fe₃O₄@ZIF-8 magnetic core-shell microspheres. The Fe₃O₄@ZIF-8 was synthesized by coating mercaptoacetic acids capped Fe₃O₄ nano-particles with ZIF-8 at room temperature. Then, a simple MSPE method for enriching five PAEs was developed with the Fe₃O₄@ZIF-8 core-shell magnetic microspheres as sorbent. Compared with previous reported extraction methods, this proposed method based on Fe₃O₄@ZIF-8 is a simpler, more rapid, and more cost-effective method for extraction of PAEs. Finally, this method was successfully applied in determination of five typical PAEs in environmental water samples.Chapter Three: Fe₃O₄@SiO₂@ZIF-8 magnetic nano-composites were prepared, and it is used as adsorbent to establish a fast and efficient method of magnetic solid phase micro-extraction. This method has several advantages of simple operation, less organic solvent consumption and high extraction efficiency. The method was successfully used for determination of UV absorber in environmental water samples.Chapter Four: A filter head based extraction method was developed with MIL-101 as the adsorbent. The optimal conditions for extration of plant growth regulators residue were systematically investigated. The residual plant growth regulators in the apple and cumber were successfully determined by combining the filter head based extraction method and HPLC with UV detection.Chapter Five: The novel filter head based extraction method was used to extract phenoxy carboxylic acids from surface water samples. The optimal conditions were obtained by single factor optimization experiments. Two kinds of phenoxy carboxylic acids herbicides residue were detected in water samples by coupling filter head based extraction method and HPLC-UV detection. It was demonstrated that the proposed method is suitable for trace analysis of phenoxy carboxylic acids from environmental water samples...