Development and evaluation of a 2D-LC-IRMS hyphenation for the use of conventional reversed-phase HPLC in compound-specific stable isotope analysis
开发和评估 2D-LC-IRMS 联用,用于在化合物特异性稳定同位素分析中使用传统反相 HPLC
基本信息
- 批准号:537343248
- 负责人:
- 金额:--
- 依托单位:
- 依托单位国家:德国
- 项目类别:Research Grants
- 财政年份:
- 资助国家:德国
- 起止时间:
- 项目状态:未结题
- 来源:
- 关键词:
项目摘要
Compound-specific stable isotope analysis (CSIA) is a method for determining the ratio of naturally occurring isotopes in single molecules. The coupling of liquid chromatography (LC) with an isotope ratio mass spectrometer (IRMS) allows the determination of carbon isotope ratios in complex samples and is used in various fields, including the determination of the origin and fate of organic pollutants in the environment and authenticity analysis in food monitoring. LC-IRMS coupling uses wet chemical oxidation of the analytes, in which all oxidisable carbon is converted to CO2. For this reason, any organic additives as eluents or buffers must be avoided as they can falsify the carbon isotope determination. However, as 90% of established LC methods use organic solvents, the application of LC-IRMS has been very limited to date. To overcome this obstacle of CSIA by LC-IRMS, the proposed project shall develop and validate the concept of two-dimensional LC (2D-LC) for stable isotope analysis. To that end, established separations from literature will be used in the first dimension that utilize organic solvents. In the second dimension, the organic solvent is separated from the analyte before the latter is oxidised to CO2 in the LC-IRMS interface. Different methods such as the sample loop method, the at-column dilution method and the trap method will be investigated. Here, the analytical parameters solvent compatibility, sensitivity and integrity of isotope signatures are the focus of the validation. Besides the separation of analytes from the solvent peak coeluting compounds from the first dimension shall also be separated by selecting suitable separation mechanisms in the second dimension. In the context of the investigation of the trap method the use of thermoresponsive phases in the trap column will be additionally investigated to allow the transfer of the analyte from 1D to 2D via a moderate temperature change. In the final part of the project, the knowledge gained will be used to demonstrate the applicability of the developed methods in various examples of the characterisation of chemical substances and transformation processes.
化合物特定稳定同位素分析(CSIA)是一种确定单分子中天然存在的同位素比例的方法。液相色谱(LC)与同位素比质谱仪(IRMS)的耦合允许测定复杂样品中的碳同位素比,并用于各种领域,包括确定环境中有机污染物的来源和归宿以及食品监测中的真实性分析。LC-IRMS偶联使用分析物的湿化学氧化,其中所有可氧化的碳转化为CO2。出于这个原因,必须避免任何有机添加剂作为洗脱液或缓冲液,因为它们可能使碳同位素测定失真。然而,由于90%已建立的LC方法使用有机溶剂,LC-IRMS的应用迄今为止非常有限。为了克服LC-IRMS CSIA的这一障碍,拟议项目将开发和验证用于稳定同位素分析的二维LC(2D-LC)概念。为此,将在利用有机溶剂的第一维中使用来自文献的已建立的分离。在第二维中,在分析物在LC-IRMS界面中氧化成CO2之前,将有机溶剂与分析物分离。将研究不同的方法,如样品定量环法、柱上稀释法和捕集器法。在此,分析参数溶剂相容性、灵敏度和同位素特征的完整性是验证的重点。除了从溶剂峰中分离分析物外,还应通过选择合适的分离机制在第二维中分离来自第一维的共洗脱化合物。在研究捕集方法的背景下,将另外研究在捕集柱中使用热敏相,以允许通过适度的温度变化将分析物从1D转移到2D。在该项目的最后一部分,所获得的知识将用于证明所开发的方法在化学物质和转化过程表征的各种示例中的适用性。
项目成果
期刊论文数量(0)
专著数量(0)
科研奖励数量(0)
会议论文数量(0)
专利数量(0)
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Professor Dr. Torsten Schmidt其他文献
Professor Dr. Torsten Schmidt的其他文献
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