Mazarin Michaël, Viel Stéphane, Allard-Breton Béatrice, Thévand André, Charles Laurence
JE 2421 TRACES (Théorie, Recherche et Applications Concertées en Spectrométries), Universités Aix Marseille I & III, Faculté de Saint-Jérôme, Service 511, 13397 Marseille Cedex 20, France.
Anal Chem. 2006 Apr 15;78(8):2758-64. doi: 10.1021/ac0522207.
This study shows how mass spectrometry and pulsed gradient spin-echo (PGSE) nuclear magnetic resonance can be advantageously combined to achieve more reliable molecular weight information for polymers. Specifically, PGSE was shown to be a convenient tool for a rapid evaluation of Mw values to be further used as guidelines in matrix-assisted laser desorption/ionization (MALDI) sample preparation. PGSE calibration curves, established under given experimental conditions, were shown to be particularly robust, as they could be applied satisfactorily on different commonly available NMR instruments and different time frames. PGSE results were shown to compare well with size exclusion chromatography data used as a reference to validate this alternative technique. Moreover, because PGSE is relatively fast, it can be used interactively with MALDI analysis to check and understand mass spectrum profiles. This approach was first tested on poly(methyl methacrylate) (PMMA) standards and then successfully applied to determine the molecular weight of two unknown samples, a PMMA and a poly(ethylene glycol) monomethacrylate polymer.
本研究展示了如何将质谱法与脉冲梯度自旋回波（PGSE）核磁共振法有效结合，以获取更可靠的聚合物分子量信息。具体而言，PGSE被证明是一种便捷工具，可快速评估Mw值，进而作为基质辅助激光解吸/电离（MALDI）样品制备的指导。在给定实验条件下建立的PGSE校准曲线显示出特别的稳健性，因为它们可以令人满意地应用于不同的常用核磁共振仪器和不同的时间范围。PGSE结果与用作参考以验证这种替代技术的尺寸排阻色谱数据相比表现良好。此外，由于PGSE相对快速，它可以与MALDI分析交互使用，以检查和理解质谱图。这种方法首先在聚甲基丙烯酸甲酯（PMMA）标准品上进行测试，然后成功应用于测定两个未知样品的分子量，一个是PMMA，另一个是聚乙二醇单甲基丙烯酸酯聚合物。
