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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Stir bar sorptive extraction with gas chromatography-mass spectrometry for the determination of resveratrol, piceatannol and oxyresveratrol isomers in wines
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Stir bar sorptive extraction with gas chromatography-mass spectrometry for the determination of resveratrol, piceatannol and oxyresveratrol isomers in wines

机译:气相色谱-质谱法搅拌棒吸附萃取法测定葡萄酒中的白藜芦醇,苦味酚和氧白藜芦醇异构体

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摘要

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 0.2-1.0μgL~(-1) concentration range, depending on the compound. The main compound determined in the analyzed samples was trans-resveratrol, with concentrations in the range of 3-230μgL~(-1), depending on the type of wine.
机译:优化了一种基于搅拌棒吸附萃取和气相色谱-质谱联用的热脱附装置(SBSE-TD-GC-MS)的简单且高度灵敏的方法,用于测定白藜芦醇的苦味酚,甲基邻苯三酚和葡萄酒样品中的氧化白藜芦醇。顺式异构体的定量是通过将相应的反式物种预先浓缩到SBSE萃取相中而生成的,从而进行的。考虑到要考虑的大量变量,使用Plackett-Burman设计研究了乙酰化衍生化,SBSE提取和热脱附步骤的优化。使用双酚F作为内标可以根据水标对样品进行定量。以10次连续分析的相对标准偏差表示的可重复性在5%至9%之间,这确认了在优化条件下可获得的高精度。对于0.2-1.0μgL〜(-1)浓度范围内的加标样品,根据化合物的不同,回收率可达到79%至109%。分析样品中确定的主要化合物为反式白藜芦醇,其浓度范围为3-230μgL〜(-1),具体取决于葡萄酒的类型。

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