Dienstleistungszentrum Ländlicher Raum (DLR) Rheinpfalz, Competence Centre for Wine Research, Breitenweg 71, D-67435 Neustadt an der Weinstrasse, Germany.
J Chromatogr A. 2013 Jan 4;1271(1):181-4. doi: 10.1016/j.chroma.2012.11.020. Epub 2012 Nov 19.
A robust method for routine quality control of corky off-flavour compounds in wine and cork soak matrices has been established. Based on an automated headspace solid phase microextraction (HS-SPME), the method needs only marginal sample preparation and achieves low (sub-ng L(-1)) trace level detection limits (LODs) for the most relevant off-flavour compounds, such as 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA) and 2,4,6-tribromoanisole (TBA). Particularly for wine matrix, reliable trace level quantification had only been achieved after applying heart-cutting multidimensional gas chromatography (MDGC). Using a halogen-sensitive electron capture detector (ECD) and quantification with a stable isotope dilution assay (SIDA), LODs of 0.1ng L(-1) for TCA, TeCA and TBA could be obtained. Since a SIDA based quantification method is used with a non-mass spectrometric detector, the necessary chromatographic resolution of internal standard and target analyte peaks resulted from the use of highly deuterated [(2)H(5)]-isotopologues.
已建立一种用于葡萄酒和软木塞浸提液中木塞味化合物常规质量控制的稳健方法。基于自动化顶空固相微萃取（HS-SPME），该方法仅需要少量的样品制备，并且可以实现最相关异味化合物（如 2,4,6-三氯苯甲醚（TCA）、2,3,4,6-四氯苯甲醚（TeCA）和 2,4,6-三溴苯甲醚（TBA））的低（亚纳克每升（ng L(-1)））痕量检测限（LOD）。特别是对于葡萄酒基质，仅在应用切心多维气相色谱（MDGC）后才能实现可靠的痕量定量。使用卤化物敏感电子捕获检测器（ECD）和稳定同位素稀释分析（SIDA）定量，可获得 TCA、TeCA 和 TBA 的 LOD 分别为 0.1ng L(-1)。由于使用非质谱检测器进行 SIDA 定量方法，因此必须对来自高度氘化 [（2）H（5）] 同位素标记物的内标和目标分析物峰进行色谱分辨率。
