Ezquerro Oscar, Garrido-López Alvaro, Tena María Teresa
Chemistry Department, University of La Rioja, C/Madre de Dios 51, E-26006, Logroño La Rioja, Spain.
J Chromatogr A. 2006 Jan 13;1102(1-2):18-24. doi: 10.1016/j.chroma.2005.10.023. Epub 2005 Oct 28.
This paper describes the development of an analytical method consisting of pressurised fluid extraction (PFE) and gas chromatography-mass spectrometry (GC-MS) using experimental designs to determine two volatile compounds in naturally-tainted cork stoppers. The target analytes, 2,4,6-trichloroanisole (2,4,6-TCA) and guaiacol, are involved in the cork taint of wine. First, a Plackett-Burman experimental design was carried out in order to determine the significant experimental parameters affecting the PFE process, and then a central composite design was used to optimise these significant parameters. Once the method had been optimised, the influence of the number of extraction cycles was studied. The method was applied to determine the concentration of 2,4,6-TCA and guaiacol in three cork samples, and the results were compared with the ones obtained by multiple headspace-solid-phase microextraction (MHS-SPME) and by Soxhlet extraction.
本文描述了一种分析方法的开发，该方法由加压流体萃取（PFE）和气相色谱-质谱联用（GC-MS）组成，采用实验设计来测定天然受污染软木塞中的两种挥发性化合物。目标分析物2,4,6-三氯苯甲醚（2,4,6-TCA）和愈创木酚与葡萄酒的软木塞污染有关。首先，进行了Plackett-Burman实验设计，以确定影响PFE过程的重要实验参数，然后使用中心复合设计来优化这些重要参数。该方法优化后，研究了萃取循环次数的影响。将该方法应用于测定三个软木塞样品中2,4,6-TCA和愈创木酚的浓度，并将结果与通过多次顶空-固相微萃取（MHS-SPME）和索氏提取获得的结果进行比较。
