A pre-column fluorescent derivatization method based on nitrone formation has been applied to determine furfurals (e.g. furfural (F), 5-methyfurfural (5-MF) and 5-hydroxymethylfurfural (5-HMF)) in food samples for the first time. An N-substituted hydroxylamine reagent 4-((hydroxyamino)butyl)-7-hydroxycoumarin (HAHC) was used to react with the aldehyde group of furfurals to form stable nitrone derivatives with high fluorescence intensities. The reactions proceeded under mild conditions in 30 min with high derivatization yields (>93%). A baseline-separation of three furfurals derivatives was subsequently achieved within 25 min on a reversed-phase column. The detection limits were at the low femtomol level (S/N = 3, 20 μL per injection). The linear range of the calibration curve was 0.4-4000 nM with good correlation coefficients (R2 ≥ 0.9991). The proposed method was further applied for food sample analysis, such as bovine milk powder and raisin. Satisfactory recoveries were obtained in the range of 94.7%-103.5%. Above all, this pre-column derivatization method is simple, fast and highly sensitive, providing an effective and promising way for future studies of aldehydes in different matrices.

中文翻译：

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醛类检测的高灵敏度方法：在葡萄干和牛乳粉中糠醛分析中的应用

首次应用基于硝酮形成的柱前荧光衍生方法测定食品样品中的糠醛（例如糠醛 (F)、5-甲基糠醛 (5-MF) 和 5-羟甲基糠醛 (5-HMF)）。N-取代的羟胺试剂 4-((羟基氨基) 丁基)-7-羟基香豆素 (HAHC) 用于与糠醛的醛基反应，形成具有高荧光强度的稳定硝酮衍生物。反应在温和条件下在 30 分钟内进行，衍生收率高（> 93%）。随后在反相柱上在 25 分钟内实现了三种糠醛衍生物的基线分离。检测限处于低飞摩尔水平（S/N = 3，每次注射 20 μL）。校准曲线的线性范围为 0.4-4000 nM，具有良好的相关系数 (R2 ≥ 0.9991)。所提出的方法进一步应用于食品样品分析，例如牛奶粉和葡萄干。在 94.7%-103.5% 的范围内获得了令人满意的回收率。最重要的是，这种柱前衍生方法简单、快速且灵敏度高，为未来不同基质中醛的研究提供了一种有效且有前景的方法。