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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation
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An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

机译:基于离子对微萃取的在线联用气相色谱/质谱联用内衬衍生化分析血浆中酚酸的自动化方法

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摘要

A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing 'Micro-extraction in packed sorbent' (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve extraction yields of the more polar analytes and as the methyl donor in the automated in-liner derivatisation method. In this way, a fully automated procedure for the extraction, derivatisation and injection of a wide range of phenolic acids in plasma samples has been obtained. An extensive optimisation of the extraction and derivatisation procedure has been performed. The entire method showed excellent repeatabilities of under 10% and linearities of 0.99 or better for all phenolic acids. The limits of detection of the optimised method for the majority of phenolic acids were 10. ng/mL or lower with three phenolic acids having less-favourable detection limits of around 100. ng/mL. Finally, the newly developed method has been applied in a human intervention trial in which the bioavailability of polyphenols from wine and tea was studied. Forty plasma samples could be analysed within 24. h in a fully automated method including sample extraction, derivatisation and gas chromatographic analysis.
机译:提出了一种基于离子对“填充吸附剂中的微萃取”(MEPS)在线耦合到线性衍生化-气相色谱-质谱(GC-MS)的血浆中酚酸分析的新方法。离子对试剂具有双重作用。它既可用于提高极性较大的分析物的提取率,又可作为自动内衬衍生化方法中的甲基供体。以这种方式,已经获得了用于提取,衍生化和注射血浆样品中多种酚酸的全自动程序。提取和衍生化过程已进行了广泛的优化。整个方法对所有酚酸均显示出低于10%的出色重复性和0.99或更高的线性。大多数酚酸的优化方法的检出限为10 ng / mL或更低,而三种酚酸的检出限为100. ng / mL左右。最后,新开发的方法已应用于人体干预试验中,其中研究了葡萄酒和茶中多酚的生物利用度。可以在24小时内以全自动方法分析40个血浆样品,包括样品提取,衍生化和气相色谱分析。

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