Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum" University of Murcia, E-30100 Murcia, Spain.
J Chromatogr A. 2013 Nov 8;1315:21-7. doi: 10.1016/j.chroma.2013.09.045. Epub 2013 Sep 18.
A simple and highly sensitive procedure based on stir bar sorptive extraction coupled to gas chromatography-mass spectrometry by means of a thermal desorption unit (SBSE-TD-GC-MS) has been optimized for the determination of cis/trans isomers of resveratrol, piceatannol and oxyresveratrol in wine samples. Quantification of the cis-isomers was carried out by generating the standards from the corresponding trans-species once they had been preconcentrated on the SBSE extracting phase. The optimization of the acetylation derivatization, SBSE extraction and thermal desorption steps was investigated using Plackett-Burman designs, taking into account the high number of variables to be considered. The use of bisphenol F as internal standard allowed quantification of the samples against aqueous standards. Repeatability, expressed as relative standard deviation of 10 successive analyses was between 5% and 9%, confirming the high precision attained under the optimized conditions. Satisfactory recovery values of between 79% and 109% were obtained for spiked samples in the 0.2-1.0 μgL(-1) concentration range, depending on the compound. The main compound determined in the analyzed samples was trans-resveratrol, with concentrations in the range of 3-230 μgL(-1), depending on the type of wine.
基于搅拌棒吸附萃取（SBSE）结合热解吸单元（TD）的气相色谱-质谱联用（GC-MS）技术，建立了一种简单、高灵敏度的检测方法，用于测定葡萄酒样品中白藜芦醇、白皮杉醇和氧白藜芦醇的顺/反异构体。通过将相应的反式异构体预浓缩在 SBSE 萃取相中，从它们生成标准品，实现了顺式异构体的定量分析。采用 Plackett-Burman 设计对乙酰化衍生化、SBSE 萃取和热解吸步骤进行了优化，考虑到需要考虑的变量数量较多。使用双酚 F 作为内标，允许用水溶液标准品对样品进行定量分析。在优化条件下，10 次连续分析的相对标准偏差在 5%至 9%之间，表明精密度较高。在 0.2-1.0 μgL(-1)浓度范围内，加标样品的回收率在 79%至 109%之间，具体取决于化合物。在分析的样品中，含量最高的化合物为反式白藜芦醇，浓度范围为 3-230 μgL(-1)，具体取决于葡萄酒的类型。
