University of Marburg, Institute of Analytical Chemistry, D-35032 Marburg, Germany.
J Chromatogr A. 2012 Oct 19;1260:9-15. doi: 10.1016/j.chroma.2012.08.050. Epub 2012 Aug 23.
A method for the ultra trace analysis of 21 fluorobenzoic acids (FBAs) via GC-MS based on solid-phase extraction (SPE) and derivatization with BF3·MeOH is described. All fluorobenzoic acids were enriched and determined simultaneously. Solid-phase extraction on hydrophilic-lipophilic-balanced reversed-phase cartridges containing a poly(divinylbenzene-co-N-vinylpyrrolidone) polymer allowed a 250-fold enrichment of the acids if 100mL sample volume is used with extraction efficiencies between 71% and 94%. The method enables the determination of fluorobenzoic acid methyl esters (FBAMEs) down to the range of 6-44 ng L(-1) combined with a fast and easy sample-preparation (pH-adjusting prior to SPE and derivatization within 24 h at 64 °C directly in the vial). It uses low amounts of chemicals and is adaptable to larger and smaller sample volumes. Simultaneous extraction and determination of 21 fluorinated aromatic acids in reservoir samples with high salinity confirmed the applicability and reproducibility of the method.
本文描述了一种通过固相萃取(SPE)和 BF3·MeOH 衍生化,结合 GC-MS 对 21 种氟苯甲酸(FBAs)进行痕量分析的方法。所有的氟苯甲酸都被同时富集和测定。亲水-疏水平衡反相柱上的固相萃取,其中含有聚(二乙烯基苯-co-N-乙烯基吡咯烷酮)聚合物,如果使用 100mL 样品体积,则可以将酸富集 250 倍,萃取效率在 71%至 94%之间。该方法能够测定氟苯甲酸甲酯(FBAMEs),其浓度范围为 6-44ngL(-1),结合了快速简便的样品制备方法(在 SPE 之前调节 pH 值,在 64°C 下直接在小瓶中衍生化,24 小时内完成)。该方法使用的化学物质较少,适用于较大和较小的样品体积。在高盐度水库样品中同时提取和测定 21 种氟化芳香酸,证实了该方法的适用性和重现性。