流动注射及高效液相色谱与等离子质谱联用在铂元素总量和溴、碘形态分析中的应用

【作者】 韩旭；

【导师】 徐子刚；

【作者基本信息】 浙江大学 ， 应用化学， 2013， 硕士

【摘要】 随着现代科学技术的不断发展,人们对分析化学的要求不仅仅包括对元素总量的测定分析,同时,还十分注重对元素不同形态的分析研究。在生物、环保、临床医学、毒理学等各个领域中,元素的化学活性、生物活性及毒性等行为效应已不仅仅取决于该元素的总量,也取决于其一定的存在形态。本论文通过大量实验,研究了流动注射及高效液相色谱与等离子体质谱联用在元素总量和形态分析中的应用。第一章综述了流动注射与等离子体质谱联用的研究进展,和用于生物样品元素含量测定的应用举例,以及高效液相色谱与等离子体质谱联用测定溴、碘元素的分析方法和研究进展。第二章介绍了微流动注射进样-加热雾室-等离子体质谱联用技术成功应用于测定血清中铂元素的方法,实验中雾化室内径和长度分别为9mm和6cm,加热温度为90℃、采样环体积为5μL时得到了较佳的信号强度,实验结果令人满意。第三章对紫菜样品中的溴元素形态进行了初步研究。采用高效液相色谱与等离子体质谱联用技术,以四丁基氢氧化铵为离子对试剂,硫代硫酸钠为洗脱剂,在4min内分离并测定了紫菜样品中的溴离子和溴酸根。第四章对海水和紫菜样品中的碘形态进行了分析研究。采用高效液相色谱与等离子体质谱联用技术,以四乙基氢氧化铵为离子对试剂,苯丙氨酸为洗脱剂,在5min内分离并测定了海水及紫菜样品中的碘离子、碘酸根、一碘代酪氨酸和二碘代酪氨酸。论文的研究表明：对元素的含量进行化学分析时,除了进行元素总量的测定之外,对其进行形态分析也是十分有必要的。将流动注射及高效液相色谱与等离子体质谱联用技术应用于元素的总量和形态分析中,具有十分重要的意义。更多还原

【Abstract】 With the development of modern science and technology, the requirements of people about analytical chemistry are not only confined to determine the total amount of element, but pay great attention to the speciation analysis of element. In biological, environmental protection, clinical medicine, toxicology, and other areas, the chemical activity, biological activity and toxicity of elements depend on the total amount, as well as the speciation. The application of flow injection/high performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry in total analysis and elemental speciation analysis were studied in this paper.In chapter1, the application of flow injection with inductively coupled plasma mass spectrometry in total amount of element was introduced. Also, the advances in research on speciation analysis of iodine and bromine by high performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry were reviewed.In chapter2, a heated single pass spray chamber-based microscale flow injection sampling system was developed for the analysis of platinum in serum samples by inductively coupled plasma mass spectrometry. The maximum intensity was obtained using the single pass spray chamber with an inner diameter of9mm and a length of6cm for the heated section. When it was heated up to90℃and the sampling loop volume was selected to be5μL, a signal peak with good configuration was obtained. Satisfactory experimental results were got.In chapter3, speciation analysis for bromine in seaweed samples was studied. BrO3-and Br-were separated within4min by reversed phase high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry (RP-HPLC-ICP-MS), with tetrabutylammonium hydroxide as the ion-pair reagent and sodium thiosulfate as the eluant.In chapter4, speciation analysis for iodine in seaweed and seawater samples was studied. IO3-, I-,3-iodotyrosine (MIT) and3,5-diiodotyrosine (DIT) were separated within5min by RP-HPLC-ICP-MS, with tetraethylammonium hydroxide as the ion-pair reagent and phenylalanine as the eluant. It is necessary to determine the total amount of element, as well as the speciation analysis. Application of flow injection/high performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry in total analysis and element speciation analysis is of great significance.更多还原