Centre for Analysis and Synthesis, Department of Chemistry, Lund University, Sweden.
J Chromatogr A. 2012 Aug 3;1249:48-53. doi: 10.1016/j.chroma.2012.06.039. Epub 2012 Jun 21.
A method based on three-phase hollow fiber liquid phase microextraction was developed and successfully applied to aerosols for the analysis of lignin pyrolysis acids such as syringic acid, vanillic acid and p-salicylic acid. Important parameters related to extraction process like organic solvent for membrane phase, tri-n-octylphosphine (TOPO) oxide contents in organic solvent, stirring speed, extraction time etc. were optimized. 6-Undecanone with 15% TOPO contents (w/v) was found a suitable solvent for organic liquid membrane, 900 rpm was the optimum stirring speed and time of 4h was found optimum extraction time. Donor phase pH was 1.3 while acceptor phase pH was adjusted to 9.5. The optimized extraction method was used for the extraction of real aerosol samples. Analytes were derivatized using BSTFA containing 1% trimethylsilyl chloride and gas chromatography mass spectrometry was used for analysis. Very low limits of detection in the range 0.2-1.0 ng L(-1) were found, corresponding to 10-50 pg m(-3) of analytes in aerosols. Extraction efficiency obtained ranged 60.3-71.7% and enrichment factors ranged 3015-3585 times. The optimized method was successfully applied to aerosol samples and all of the selected analytes were detected in the analyzed samples.
建立了一种基于三相中空纤维液相微萃取的方法，并成功地将其应用于分析木质素热解酸（如丁香酸、香草酸和对羟基苯甲酸）的气溶胶。优化了与萃取过程相关的重要参数，如膜相有机溶剂、有机溶剂中三辛基氧化膦（TOPO）的含量、搅拌速度、萃取时间等。发现 6-十一酮（15%TOPO 含量，w/v）是一种适合有机液体膜的溶剂，900rpm 是最佳搅拌速度，4h 是最佳萃取时间。供体相 pH 值为 1.3，而受体相 pH 值调至 9.5。优化后的萃取方法用于真实气溶胶样品的萃取。使用含有 1%三甲基氯硅烷的 BSTFA 将分析物衍生化，并使用气相色谱-质谱法进行分析。发现检测限非常低，范围在 0.2-1.0ng/L 之间，相当于气溶胶中分析物的浓度为 10-50pg/m3。萃取效率在 60.3-71.7%之间，富集因子在 3015-3585 倍之间。优化后的方法成功地应用于气溶胶样品，并在分析样品中检测到所有选定的分析物。
