Department of Chemistry, Humboldt-University, Brook-Taylor-Str. 2, D-12489 Berlin, Germany.
Talanta. 2010 Jun 30;82(1):143-50. doi: 10.1016/j.talanta.2010.04.011. Epub 2010 Apr 18.
Commercially available linear alkylbenzenesulfonates (LASs) are a mixture of various homologues and isomers, leading to 20 major species. In this work we investigated the commercial product by liquid chromatography-solid phase extraction-nuclear magnetic resonance spectroscopy-mass spectrometry (LC-SPE-NMR/MS). The commercial product was separated into 17 fractions by liquid chromatography (LC). After chromatographic separation, 5% of the flow was split to a mass spectrometer (MS) while 95% was send to post-column solid phase extraction cartridges for enrichment of the analytes (LC-SPE). After elution from the SPE-cartridges a NMR-spectrometer equipped with a cryo-probe was used for the characterisation of the different LASs species. For the first time (1)H-1D and H-H-COSY spectra for 14 LASs species out of 20 major isomers are presented, whereas the 6 remaining species are detected as mixtures in 3 (1)H-1D and H-H-COSY spectra. These data were used to correlate the chromatographic retention of the LASs isomers to the substitution pattern of the alkyl chain.
市售直链烷基苯磺酸盐（LAS）是各种同系物和异构体的混合物，导致 20 种主要物质。在这项工作中，我们通过液相色谱-固相萃取-核磁共振波谱-质谱法（LC-SPE-NMR/MS）研究了商业产品。商业产品通过液相色谱（LC）分离成 17 个馏分。色谱分离后，5%的流量被分流到质谱仪（MS），而 95%的流量被发送到柱后固相萃取小柱中以富集分析物（LC-SPE）。从小柱洗脱后，使用配备低温探头的核磁共振波谱仪对不同 LAS 物质进行了表征。首次（1）H-1D 和 H-H-COSY 谱图呈现了 20 种主要异构体中的 14 种 LAS 物质，而其余 6 种物质在 3 个（1）H-1D 和 H-H-COSY 谱图中被检测为混合物。这些数据被用来将 LAS 异构体的色谱保留与烷基链的取代模式相关联。
