Insa S, Anticó E, Ferreira V
Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona, Spain.
J Chromatogr A. 2005 Sep 30;1089(1-2):235-42. doi: 10.1016/j.chroma.2005.06.061.
A reliable solid-phase extraction (SPE) method for the simultaneous determination of 2,4,6-trichloroanisole (TCA) and 2,4,6-tribromoanisole (TBA) in wines has been developed. In the proposed procedure 50 mL of wine are extracted in a 1 mL cartridge filled with 50 mg of LiChrolut EN resins. Most wine volatiles are washed up with 12.5 mL of a water:methanol solution (70%, v/v) containing 1% of NaHCO3. Analytes are further eluted with 0.6 mL of dichloromethane. A 40 microL aliquot of this extract is directly injected into a PTV injector operated in the solvent split mode, and analysed by gas chromatography (GC)-ion trap mass spectrometry using the selected ion storage mode. The solid-phase extraction, including sample volume and rinsing and elution solvents, and the large volume GC injection have been carefully evaluated and optimized. The resulting method is precise (RSD (%) < 6% at 100 ng L(-1)), sensitive (LOD were 0.2 and 0.4 ng/L for TCA and TBA, respectively), robust (the absolute recoveries of both analytes are higher than 80% and consistent wine to wine) and friendly to the GC-MS system (the extract is clean, simple and free from non-volatiles).
已开发出一种可靠的固相萃取（SPE）方法，用于同时测定葡萄酒中的2,4,6 - 三氯苯甲醚（TCA）和2,4,6 - 三溴苯甲醚（TBA）。在所提出的方法中，将50 mL葡萄酒在装有50 mg LiChrolut EN树脂的1 mL小柱中进行萃取。用12.5 mL含有1% NaHCO₃的水：甲醇溶液（70%，v/v）冲洗掉大部分葡萄酒挥发物。用0.6 mL二氯甲烷进一步洗脱分析物。将该提取物的40 μL等分试样直接注入以溶剂分流模式运行的PTV进样器中，并通过气相色谱（GC）-离子阱质谱联用仪采用选定离子存储模式进行分析。对固相萃取，包括进样体积、冲洗和洗脱溶剂，以及大体积GC进样进行了仔细评估和优化。所得方法精确（在100 ng L⁻¹时相对标准偏差（RSD）（%）< 6%）、灵敏（TCA和TBA的检测限分别为0.2和0.4 ng/L）、稳健（两种分析物的绝对回收率均高于80%且不同葡萄酒之间结果一致）且对GC - MS系统友好（提取物干净、简单且无挥发性杂质）。
