A GC/MS based method for the thorough analysis of sterols in food

基于 GC/MS 的方法用于彻底分析食品中的甾醇

• 批准号: 450537549
• 负责人: Professor Dr. Walter Vetter
• 金额: --
• 依托单位: Institut für Lebensmittelchemie (170)
• 依托单位国家: 德国
• 项目类别: Research Grants
• 财政年份: 2020
• 资助国家: 德国
• 起止时间: 2019-12-31 至 2023-12-31
• 项目状态: 已结题
• 来源: https://gepris.dfg.de/gepris/projekt/450537549?language=en
• 关键词: GC; MS; based; method; thorough

Sterols are bioactive lipid compounds virtually found in all food samples at concentrations of ~1% of the total lipids. This substance class exists in a variety of over 250 individual compounds. However, very few are available as reference standards, and less than 20 can be measured in routine analysis by existing routine methods. During the analysis of samples, many of the sterols are overlooked, and labelled unknown or wrongly. In addition, determination of minor sterols was reported to be prone to errors. The goal of this project is the development of a sensitive GC/MS method that allows the thorough analysis of all sterols in and from food samples. For this purpose, a new concept based on Kováts indices was developed using self-synthesized fatty acid pyrrolidine esters (pyrrolidides) as reference compounds in combination with a highly sensitive GC/MS selected ion monitoring (SIM) screening method that allows to assign structures to trace sterols (contribution <0.01% to the lipids). Tentatively identified sterols will be enriched/isolated by means of countercurrent chromatography (CCC) and other methods (hydrogenation, solid phase extraction) followed by structure investigation by GC/MS and NMR. Several deuterium labelled compounds will be synthesized for use as internal standards for quantification. All data will be merged in a comprehensive data base that will allow users to determine sterols reliably for different purposes.

硬脂酸是一种生物活性脂质化合物，几乎存在于所有食物样品中，浓度约为总脂质的1%。该物质类别存在于250多种单独的化合物中。然而，很少有可作为参考标准，并且通过现有的常规方法在常规分析中可以测量不到20个。在样品分析过程中，许多甾醇被忽视，并标记为未知或错误。此外，据报道，测定次要甾醇容易出错。该项目的目标是开发一种灵敏的GC/MS方法，可以彻底分析食品样品中的所有甾醇。为此，开发了一种基于Kováts指数的新概念，使用自行合成的脂肪酸吡咯烷酯（吡咯烷）作为参比化合物，结合高灵敏度的GC/MS选择离子监测（SIM）筛选方法，可以将结构分配给痕量甾醇（对脂质的贡献<0.01%）。暂时鉴定的甾醇将通过逆流色谱法（CCC）和其他方法（氢化，固相萃取）富集/分离，然后通过GC/MS和NMR进行结构研究。将合成几种氘标记的化合物，用作定量的内标。所有数据将合并在一个全面的数据库，使用户能够确定甾醇可靠的不同用途。