| Since the novel M41S mesoporous materials (particularly MCM-41) was firstly reported by Mobil's researchers, much attention has been paid to this kind of materials. They have not only larger surface area, uniform pore structure and huge pore volume, which can reduce bottleneck phenomenon in molecular diffusion, but also higher mechanically and chemically stability as new inorganic materials. These materials have been widely used as catalysts, sorbents and separation materials as they were synthesized firstly. Especially, the mesoporous materials with functionalization and various morphologies have been developed in order to obtain higher selectivity and special action sites in past decades.At the same time, solid-phase microextraction (SPME) as a new solvent-free extraction technique in sample preparation appeared in early 1990s. Because of its advantages of simplicity, rapid extraction and easy quantification, SPME was successfully applied to extraction and concentrating of many compounds in environment, food, biological fluids and pesticide matrices, the samples included gas, liquid and solid. SPME could be easily utilized with gas chromatography (GC) and high performance liquid chromatography (HPLC). Latterly, it coupled with Ultraviolet Absorption Spectroscopy (UVAS), Capillary Electrophoresis (CE) and other apparatuses.Up to date, many experimental coatings were prepared and investigated for a wide range of applications. The general applications for SPME are that fused silicate fibers were coated with various liquid polymeric coatings, such as polydimethylsiloxane (PDMS) and polyacrylate (PA). Lately, other more specialized materials have been developed, including ion-exchange coatings, liquid crystalline films, carbowax and Nafion coatings. Conducting polymers, such as polypyrrole, polythiephene and polyaniline were also used as coating materials. In order to increase selectivity, polymer imprinting was also introduced to fiber coatings. Contrast to liquid polymeric coatings, solid coatings were also utilized as SPME coating, for example GBC, porous layer activated carbon (PLAC) and PVC-activated charcoal. Porous silica, especially silica bonded phases (SBP) of HPLC, was also introduced to SPME as fiber coating, which had higher extraction capacity, shorter analysis time and higher sensitivity.In this paper, we introduced novel mesoporous material C16-MCM-41 to prepare SPME fibers. Coating was prepared by fixing C16-MCM-41 particles onto the stainless steel wire. Because of C16-MCM-41 with larger surface area and uniform pore structure, the extraction capacity of coating could be greatly increased. As a result, the sensitivity of method was enhanced. The extraction efficiency, stability, selectivity and quantity capability of C16-MCM-41 coated fibers to the samples were investigated.The dissertation consists of seven parts:Chapter 1, reviews the current state of the art in mesoporous materials research, simply introduces its synthesis according to different channel structure, shape as well as derivative production. But the emphasis is focused on its application in separation science and technology, such as membrane separation, selective adsorption of gases, liquids and metal ions. The chromatographic applications for mesoporous materials are also reviewed firstly in this chapter. All of these applications are presented by elaborating. We also make an outlook to the future of mesoporous research and separation application.In Chapter 2, amino and ether organic group were successfully grafted into the pore of MCM-41 mesoporous sieve using y-aminopropyltriethoxy silane and y-glycidoxypropyltrimethoxy silane as a coupling agent. The inorganic/organic composite mesoporous materials, NH2(CH2)3-MCM-41 and CH2OCHCH2O(CH2)3-MCM-41, were synthesized, and characterized by XRD, nitrogen adsorption-desorption, elemental analysis and FT-IR..In Chapter 3, the B-CD was first successfully introduced into the pore of MCM-41 mesoporous sieve using r-glycidoxypropyltrimethoxy silane (GPTS) as a coupling...
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