Campillo Natalia, Aguinaga Nerea, Viñas Pilar, López-García Ignacio, Hernández-Córdoba Manuel
Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, E-30071 Murcia, Spain.
J Chromatogr A. 2004 Dec 17;1061(1):85-91. doi: 10.1016/j.chroma.2004.11.005.
A method based on solvent extraction and purge-and-trap capillary gas chromatography with atomic emission detection (PT-GC-AED) for the determination of 2,4,6-trichloroanisole (TCA) in wines and cork stoppers was optimized and evaluated. TCA was previously extracted from the samples in pentane and the preconcentrated extract was reconstituted in water before being injected into the chromatograph by means of the PT system. Element-specific detection and quantification was carried out by monitoring the chlorine (479 nm) emission line. Two different calibration graphs were used to quantify TCA in the cork or the wine samples, owing to the interference produced by the ethanol content in the wines. Detection limits of 25 pg g(-1) and 5 ng l(-1) were obtained for corks and wines, respectively. The method provided recoveries from spiked samples ranging from 88.5 to 102.3%, confirming the reliability of the procedure and its suitability for routine monitoring.
优化并评估了一种基于溶剂萃取和吹扫捕集毛细管气相色谱-原子发射检测（PT-GC-AED）的方法，用于测定葡萄酒和软木塞中的2,4,6-三氯苯甲醚（TCA）。TCA预先从样品中用戊烷萃取，预浓缩提取物在通过PT系统注入色谱仪之前用水复溶。通过监测氯（波长479nm）发射线进行元素特异性检测和定量。由于葡萄酒中乙醇含量产生的干扰，使用两种不同的校准曲线来定量软木塞或葡萄酒样品中的TCA。软木塞和葡萄酒的检测限分别为25 pg g(-1)和5 ng l(-1)。该方法对加标样品的回收率为88.5%至102.3%，证实了该程序的可靠性及其适用于常规监测。
