CHROMATOGRAPHY/PLASMA MASS SPECTROMETRY FOR ULTRA-TRACE ANALYSIS

用于超痕量分析的色谱/等离子体质谱法

• 批准号: 6106192
• 负责人: JOSEPH A CARUSO
• 金额: $ 17.11万
• 依托单位: UNIVERSITY OF CINCINNATI
• 依托单位国家: 美国
• 财政年份: 1999
• 资助国家: 美国
• 起止时间: 1999-04-01 至 2001-03-31
• 项目状态: 已结题
• 来源: https://reporter.nih.gov/project-details/6106192
• 关键词: arsenic; capillary electrophoresis; chromatography; chromium; electrospray ionization mass spectrometry; environmental contamination; gas chromatography; high performance liquid chromatography; ion exchange chromatography; mass spectrometry; method development; organometallic compounds

Adequate risk assessment and subsequent corrective actions will in large measure depend upon the reliability, sensitivity, efficacy and low level detection capabilities of the methods utilized for sample analysis. These levels are now possible with the chromatographic and plasma MS techniques we have been developing and are now extending plus adding new dimensions. Costs to human health plus clean and safe environment concerns easily outweigh the financial burden and strongly mandate state- of -the art research to develop accurate, precise, and robust analytical techniques with potential environmental applicability. The research proposed herein is a comprehensive approach to basic understanding and development of analytical methods for complex environmental samples. These samples, by necessity, require both separation techniques and detection methods capable of ultra-trace measurement. Extended collaborations have begun during this current project period. This project has four specific aims with the general goal to continue development of trace methods of analysis for environmentally hazardous compounds. A. Continue studies of metal speciation. We now propose to do further our studies with applications to environmental relevant "real" sample types and will involve extensive interactions with the projects by Dixon, Warshawsky, Bishop and Tabor. New applications with SFC, microbore LC, and micellar LC with ICP-MS detection will provide critical speciation information. B. Supercritical fluids for extraction (SFE) and trace level analysis (SFC). As it is critical to our studies that the original species integrity be preserved, we aim to study the use of SFE for the extraction of trace levels of various species of interest. We also will study the fundamental phase behavior of mixed solvent systems for SFE. C. Electromigration separations for improved separation selectivity. We aim to continue and expand our studies of Electromigration techniques including capillary electrophoresis (CE) and a new technique, electrochromatography coupled with our sensitive plasma mass spectrometry to allow unparalleled separation efficiency and low detection limits. Electrochromatography is a hybrid of traditional liquid chromatography and CE, which offers some of the advantages of both methods with a dramatic increase in column efficiency. D. Electrospray as a source for elemental mass spectrometry. Our aims in this project are to utilize applications to the Cr speciation problem we have been studying for several years. Depending on the Electrospray interface conditions, markedly different mass spectra can be attained from those showing extensive clustering to those showing the bare element at its characteristic mass to a high amount of speciation information at trace levels - and without the need for the plasma source.

充分的风险评估和随后的纠正行动将在很大程度上 措施取决于可靠性，敏感性，有效性和低水平 用于样品分析的方法的检测能力。 这些水平现在可以通过色谱和血浆MS 我们一直在开发的技术，现在正在扩展和添加新的 尺寸. 对人类健康以及清洁和安全环境的成本 这些问题很容易超过财政负担，并强烈要求国家- 最先进的研究，以开发准确，精确和强大的分析 具有潜在环境适用性的技术。 本文提出的研究是一个全面的方法， 理解和发展复杂的分析方法 环境样品。 这些样本，必要时，需要 超痕量的分离技术和检测方法 测量. 在这一时期，扩大合作已经开始。 项目期间。 该项目有四个具体目标， 目标是继续开发痕量分析方法， 对环境有害的化合物 A.继续研究金属 物种形成 我们现在建议进一步研究应用 环境相关的“真实的”样品类型，将涉及广泛的 与狄克逊，Warshawsky，Bishop和塔博尔的项目的互动。 SFC、微孔LC和胶束LC与ICP-MS的新应用 检测将提供关键的物种形成信息。 B。超临界 用于提取（SFE）和痕量分析（SFC）的流体。 因为它是 对我们的研究至关重要的是原始物种的完整性得到保护， 我们的目的是研究使用超临界流体萃取的痕量水平， 各种感兴趣的物种。 我们还将研究基本阶段 混合溶剂体系的行为。 C.电迁移 分离以提高分离选择性。 我们的目标是继续和 扩展了我们对电迁移技术的研究，包括毛细管 电泳（CE）和一种新技术，电色谱耦合 利用我们灵敏的等离子体质谱仪，实现无与伦比的 分离效率高，检测限低。 电色谱 是传统液相色谱和CE的混合物， 这两种方法的一些优点是显著增加了列 效率 D.电喷雾作为元素质谱的源。 我们在这个项目中的目的是利用应用程序的铬形态 这个问题我们已经研究了好几年了。 取决于 电喷雾界面条件，明显不同的质谱可以 从显示广泛聚类的那些到显示 裸元素在其特征质量到高数量的物种形成 信息在痕量水平-而不需要等离子体源。