聚n-异丙基丙烯酰胺整体柱的制备及在线分析酚类化合物-药物分析学专业论文.docx

摘要摘要酚类化合物的分析测定主要利用高效液相色谱法(HPLC)，尤其是反相高效液相色谱 法。然而，在实际样品的分离分析中，为了达到必要的灵敏度水平，在对酚类化合物测 定之前，需要将干扰色谱分析的物质去除。所以，样品前处理成为了定量分析的关键步 骤。目前，固相萃取技术已经成为一种重要的样品前处理技术。固相萃取的核心就是固 相萃取填料。近年来发展起来的有机聚合物整体柱制备方法简单、通透性高及选择性好， 成为了固相萃取很受欢迎的吸附填料。本文以 N-异丙基丙烯酰胺(NIPAAm)为单体，自制的乙烯基酯树脂为交联剂/view/450276.htm，偶氮 /view/450276.htm二异丁腈(AIBN)为引发剂，十六醇为致孔剂，甲醇为溶剂，采用自由基聚合原理在 60 °C 恒温水浴中制备 poly (NIPAAm-co-vinyl ester resin)整体柱。利用扫描电镜、红外光谱仪 对该材料的结构和官能团进行了表征。将自制整体柱连接于高效液相色谱系统中，考察 了柱背压与流速的关系，并利用该整体柱作为吸附材料，在线富集、分析了废水中的五 个酚类化合物。考察了该方法学的线性，精密度，回收率，验证了自制整体柱在废水中 的可应用性。实验结果证明，该方法具有良好的线性范围和精密度。该整体柱作为酚类 化合物的在线富集的吸附材料是可行的。关键词N-异丙基丙烯酰胺(NIPAAm)，固相萃取，高效液相色谱(HPLC)，整体柱，酚 类化合物AbstractAbstractThe normal analytical techniques used in determination of phenols is mainly high-performance liquid chromatography (HPLC), especially the reversed-phase liquid chromatography (RPLC). However, in the analysis of practical samples, in order to obtain certain sensitivity, the substances interfered to the chromatographic analysis should be removed before the determination of phenols. Thus, sample preparation is a key step in quantitative analysis.Solid phase extraction technology has become an important sample pre-treatment technology at present. Moreover, sorbent for core of the solid-phase extraction has become a critical factor. In recent years, organic polymeric monolith has become very popular for SPE due to its advantages such as easy preparation, high selectivity and high permeability.In this thesis, a porous poly (N-isopropylacrylamide-co-vinyl ester resin) [poly (NIPAAm-co-vinylesterresin)]monolithiccolumnwassynthesizedbyusing N-isopropylacrylamideasmonomer;vinylesterresinascrosslinkingagent;2, 2-azobisisobutyronitrile as initiator; cetyl alcohol as porogen; methanol as solvent. The polymerization was carried out via a free-radical polymerization technique at 60 °C. The morphology and groups of the materials were assayed by scanning electron microscopy (SEM) and FT-IR spectrum, respectively. The effects of mobile phase flow rate