Kubica Paweł, Vacchina Véronique, Wasilewski Tomasz, Reynaud Stéphanie, Szpunar Joanna, Lobinski Ryszard
Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology, Narutowicza 11/12, 80-233, Gdańsk, Poland.
UT2A, Hélioparc, 2, Avenue Pr. Angot, 64053, Pau, France.
Anal Bioanal Chem. 2017 Feb;409(4):871-879. doi: 10.1007/s00216-016-0060-5. Epub 2016 Nov 10.
A matrix removal procedure with ion-exchange resin prior to analysis for 18 fluorinated benzoic acids (FBAs) tracers in saline (>25% salt) reservoir water was optimized. The elimination of >98% of salt and the simultaneous matrix sample cleanup allowed the direct analysis using the supernatant by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). This resulted in a gain in detection limits for most of the tracers in comparison with the reference method (direct analysis after minimum required dilution). The limits of detection (LODs) were in the range of 0.01-0.15 ng/ml and compared to other studies the developed method provided comparable limits of detection and advantage of simplified and shorter sample preparation. The presented method offers a considerable gain in simplicity and analysis time. Recoveries for all the tracers reached 80-100%, except for 2-FBA and 2,6-dFBA for which they were ca. 60%. The low recoveries were corrected by the use of five isotopically labeled internal standards. The method was validated by the analysis of spiked samples and by an independent comparison of the results with those obtained by solid-phase extraction LC-MS/MS method.
对盐水(盐含量>25%)储层水中18种氟化苯甲酸(FBA)示踪剂进行分析前,优化了一种使用离子交换树脂的基质去除程序。去除了>98%的盐分,同时对基质样品进行了净化,使得能够直接使用液相色谱-串联质谱法(LC-MS/MS)对上清液进行分析。与参考方法(在进行最低限度所需稀释后直接分析)相比,这使得大多数示踪剂的检测限有所降低。检测限(LOD)在0.01 - 0.15 ng/ml范围内,与其他研究相比,所开发的方法具有相当的检测限,且具有简化和缩短样品制备过程的优势。所提出的方法在简便性和分析时间方面有显著提升。除2-FBA和2,6-dFBA的回收率约为60%外,所有示踪剂的回收率均达到80 - 100%。通过使用五种同位素标记的内标物对低回收率进行了校正。通过对加标样品的分析以及将结果与固相萃取LC-MS/MS方法获得的结果进行独立比较,对该方法进行了验证。