Riu M, Mestres M, Busto O, Guasch J
Departament de Química Analítica i Química Orgànica, Unitat d'Enologia del CeRTA, Facultat d'Enologia de Tarragona, Universitat Rovira i Virgili, 43007 Tarragona, Catalonia, Spain.
J Chromatogr A. 2006 Feb 24;1107(1-2):240-7. doi: 10.1016/j.chroma.2005.12.063. Epub 2006 Jan 6.
Chloroanisoles can migrate from the cork stopper in wine bottles to the wine and give it a musty taint so it is important to find a method by which they can be determined. The aim of this paper is to develop a method for quantifying 2,4-dichloroanisole, 2,6-dichloroanisole, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole and 2,3,4,5,6-pentachloroanisole in cork using headspace solid-phase microextraction and gas chromatography with electron capture detection. After we had prepared the cork standards that were so essential to the work we optimised the parameters that most influence headspace solid-phase microextraction: fibre coating, vial volume, cork, kind and volume of solvent to help the extraction, extraction temperature and time, ionic strength and stirring. The method quantifies the total amount of chloroanisoles in cork stoppers (natural, agglomerated, agglomerated with disks and sparkling wine stoppers), at suitable concentrations so that the capacity of these compounds to give wine a musty taint can be evaluated. The quantification limits are: 2,6-dichloroanisole (8.6 ng/g), 2,4,6-trichloroanisole (0.8 ng/g), 2,4-dichloroanisole (3.5 ng/g), 2,3,4,6-tetrachloroanisole (0.6 ng/g), 2,3,4,5,6-pentachloroanisole (0.8 ng/g). The other quality parameters are: recoveries (90.3-105.8%), repeatability (4-13% (RSD expressed)) and intermediate precision (5-14% (RSD expressed)).
氯代苯甲醚会从葡萄酒瓶的软木塞迁移至葡萄酒中，使其带有一股霉味，因此找到一种能够测定它们的方法很重要。本文的目的是开发一种采用顶空固相微萃取和带电子捕获检测的气相色谱法来定量软木塞中2,4 - 二氯苯甲醚、2,6 - 二氯苯甲醚、2,4,6 - 三氯苯甲醚、2,3,4,6 - 四氯苯甲醚和2,3,4,5,6 - 五氯苯甲醚的方法。在制备了对这项工作至关重要的软木塞标准品之后，我们优化了对顶空固相微萃取影响最大的参数：纤维涂层、样品瓶体积、软木塞、有助于萃取的溶剂种类和体积、萃取温度和时间、离子强度以及搅拌。该方法能够定量软木塞（天然软木塞、聚合软木塞、带圆盘的聚合软木塞和起泡葡萄酒软木塞）中氯代苯甲醚的总量，浓度适宜，以便能够评估这些化合物使葡萄酒产生霉味的能力。定量限分别为：2,6 - 二氯苯甲醚（8.6 ng/g）、2,4,6 - 三氯苯甲醚（0.8 ng/g）、2,4 - 二氯苯甲醚（3.5 ng/g）、2,3,4,6 - 四氯苯甲醚（0.6 ng/g）、2,3,4,5,6 - 五氯苯甲醚（0.8 ng/g）。其他质量参数为：回收率（90.3 - 105.8%）、重复性（4 - 13%（以相对标准偏差表示））和中间精密度（5 - 14%（以相对标准偏差表示））。
