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首页> 外文期刊>CHROMATOGRAPHY >Multi-Perfluoroalkyl Derivatization of Polyamines for Selective Liquid Chromatography-Tandem Mass Spectrometric Analysis Utilizing Fluorous Affinity
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Multi-Perfluoroalkyl Derivatization of Polyamines for Selective Liquid Chromatography-Tandem Mass Spectrometric Analysis Utilizing Fluorous Affinity

机译：多胺的全氟烷基的多全氟烷基衍生化，利用氟亲和力进行选择性液相色谱-串联质谱分析

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A novel derivatization method for the selective and sensitive liquid chromatography (LC)-tandem mass spectrometric (MS/MS) analysis of polyamines (putrescine, cadaverine, spermidine, and spermine) was developed. In this study, to utilize the specific affinity between perfluoroalkyl compounds, called ‘fluorous’ affinity, two to four amino groups in each polyamine molecule were transformed with a relatively short perfluoroalkyl reagent, N -succinimidyl 4,4,5,5,6,6,7,7,8,8,9,9,9-tridecafluorononanoate to achieve the corresponding diperfluoroalkyl- to tetraperfluoroalkyl-derivatives. Compared with the non-fluorous compounds, the fluorophilicity of the multi-fluorous derivatives was sufficient for realizing strong retention on an LC column with a perfluoroalkyl-modified stationary phase. Furthermore, sensitive analysis of these derivatives could be performed using the multiple reaction monitoring mode in positive electrospray ionization-MS/MS. The limits of detection of the polyamines were in the range of 0.31–1.4 nM. The method was validated using human plasma samples. Although the recoveries from spiked human plasma after ultrafiltration were in the range of 66.4–103%, the derivatives could be determined without interference from matrix effects because of their selective retention on the column, which excluded non-fluorous biological matrix components, such as phospholipids. Therefore, this sensitive and selective analysis method was useful for the determination of trace amounts of polyamines in human plasma.
机译：建立了一种新的衍生化方法，用于多胺（腐胺，尸胺，亚精胺和亚精胺）的选择性和灵敏液相色谱（LC）-串联质谱（MS / MS）分析。在这项研究中，为了利用全氟烷基化合物之间的特异性亲和力（称为“氟”亲和力），用相对较短的全氟烷基试剂N i-琥珀酰亚胺4,4,5,5转化每个多胺分子中的2-4个氨基-6,6,7,7,7,8,8,9,9,9-三氟氟壬酸酯，以实现相应的二氟烷基-四氟烷基衍生物。与非氟化合物相比，多氟衍生物的氟亲和性足以在具有全氟烷基改性固定相的LC色谱柱上实现强保留。此外，可以在正电喷雾电离-MS / MS中使用多反应监测模式对这些衍生物进行敏感分析。多胺的检出限为0.31–1.4 nM。使用人血浆样品验证了该方法。尽管超滤后从加标的人体血浆中回收的回收率在66.4％至103％之间，但由于它们在色谱柱上的选择性保留，因此可以确定这些衍生物而不受基质效应的干扰，这些衍生物排除了非氟生物基质成分，例如磷脂。因此，这种灵敏而选择性的分析方法可用于测定人血浆中的痕量多胺。

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