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搅拌棒吸附萃取-气相色谱-质谱法测定葡萄酒中白藜芦醇、皮考汀醇和氧白藜芦醇异构体

Stir bar sorptive extraction with gas chromatography-mass spectrometry for the determination of resveratrol, piceatannol and oxyresveratrol isomers in wines.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, Regional Campus of International Excellence "Campus Mare Nostrum" University of Murcia, E-30100 Murcia, Spain.

出版信息

J Chromatogr A. 2013 Nov 8;1315:21-7. doi: 10.1016/j.chroma.2013.09.045. Epub 2013 Sep 18.

Abstract

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.

摘要

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。

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