Abstract A simple and sensitive method for the simultaneous determination of glyoxal and methylglyoxal in alcoholic beverages and fermented foods was developed. This method involved simultaneous derivatization in solution with 2,2,2-trifluoroethyl hydrazine (TFEH) and headspace solid phase microextraction, followed by detection via gas chromatography-mass spectrometry (GC–MS). The method established herein can be summarized as follows. The sample was adjusted to pH 6.0 in a headspace vial, saturated with sodium chloride, and allowed to react with TFEH at 85 °C for 20 min. The formed derivatives were vaporized and adsorbed on divinylbenzene/carboxy/polydimethylsiloxane fibers. The TFEH derivatives were subsequently desorbed and analyzed by GC–MS, where the spectrum showed a single sharp peak. Under the established conditions, the quantification limits of glyoxal and methylglyoxal were 3.6 and 2.1 μg kg−1, respectively, and the relative standard deviations were under 8% at concentrations of 20, 100 and 2000 μg kg−1. All samples were detectable at typical glyoxal (62–4116 μg kg−1) and methylglyoxal (11–2342 μg kg−1) concentrations in beverages and foods.

中文翻译：

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顶空固相微萃取和气相色谱-质谱法在溶液中衍生化和检测酒精饮料和发酵食品中的乙二醛和甲基乙二醛

摘要 建立了一种同时测定酒精饮料和发酵食品中乙二醛和甲基乙二醛的简便、灵敏的方法。该方法包括在溶液中用 2,2,2-三氟乙基肼 (TFEH) 和顶空固相微萃取同时衍生化，然后通过气相色谱-质谱法 (GC-MS) 进行检测。本文建立的方法可概括如下。将样品在顶空小瓶中调节至 pH 6.0，用氯化钠饱和，并在 85 °C 下与 TFEH 反应 20 分钟。形成的衍生物被蒸发并吸附在二乙烯基苯/羧基/聚二甲基硅氧烷纤维上。TFEH 衍生物随后被解吸并通过 GC-MS 进行分析，其中光谱显示一个尖锐的峰。在既定条件下，乙二醛和甲基乙二醛的定量限分别为 3.6 和 2.1 μg kg-1，浓度为 20、100 和 2000 μg kg-1 时的相对标准偏差低于 8%。所有样品都可以检测到饮料和食品中典型的乙二醛 (62-4116 μg kg-1) 和甲基乙二醛 (11-2342 μg kg-1) 浓度。