Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, 18071 Granada, Spain.
J Chromatogr A. 2013 Nov 8;1315:1-7. doi: 10.1016/j.chroma.2013.09.028. Epub 2013 Sep 13.
A new sensitive multiresidue method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has been developed for the detection, confirmation and quantification of twenty five carbamates in wine samples. The separation was achieved in 5.5 min, using a Zorbax Eclipse plus RRHD C18 column (50 mm×2.1 mm, 1.8 μm), with a mobile phase of water and methanol, both of them with 0.01% formic acid. The analytes were detected in positive mode with multiple reaction monitoring mode. Ultrasound-assisted surfactant-enhanced emulsification microextraction (UASEME), using a low-density extraction solvent has been optimized for the satisfactory extraction of carbamates and clean-up of extracts. The matrix effect was studied, showing that the proposed procedure provides very clean extracts. Under optimum conditions, recoveries for fortified wine samples ranged from 74 to 102%, with relative standard deviations lower than 6%. Limits of quantification ranged from 0.15 to 0.92 μgl(-1), showing the high sensitivity of this fast and simple method and its compliance with current requirements.
建立了一种基于超高效液相色谱-串联质谱（UHPLC-MS/MS）的新的、灵敏的多残留方法，用于检测、确证和定量葡萄酒样品中的二十五种氨基甲酸酯。在 5.5 分钟内，使用 Zorbax Eclipse plus RRHD C18 柱（50mm×2.1mm，1.8μm），以水和甲醇为流动相，均含有 0.01%甲酸，实现了分离。采用正离子多反应监测模式检测分析物。采用超声辅助表面活性剂增强乳液微萃取（UASEME），使用低密度萃取溶剂，对氨基甲酸酯进行了满意的萃取和提取物的净化。研究了基质效应，结果表明，所提出的方法提供了非常干净的提取物。在最佳条件下，加标葡萄酒样品的回收率在 74%至 102%之间，相对标准偏差低于 6%。定量限范围为 0.15 至 0.92μg/L，表明该快速简单方法具有较高的灵敏度，符合现行要求。
