Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, University of Santiago de Compostela, 15782, Spain; Health Research Institute of Santiago de Compostela (IDIS), University of Santiago de Compostela, 15782, Spain.
Department of Analytical Chemistry, Nutrition and Food Science, Faculty of Chemistry, University of Santiago de Compostela, 15782, Spain.
Food Chem. 2022 Aug 1;384:132530. doi: 10.1016/j.foodchem.2022.132530. Epub 2022 Feb 21.
A new, fast, simple, and effective ultrasound-assisted dispersive liquid-liquid microextraction procedure (UA-DLLME) for the gas chromatography-mass spectrometry (GC-MS) determination of malondialdehyde, acrolein, and 4-hydroxy-2-nonenal in beverages was successfully developed. 2,4-Dinitrophenylhydrazine derivatization was performed during extraction. An asymmetrical 34//18 screening design and a central composite surface response design were used to investigate the influence of the most critical factors during the extraction process (ultrasound time and temperature, extraction and disperser solvents volumes, salt addition, and derivatization reagent concentration). According to FDA guidelines, the method was validated, achieving good linearities with r ≥ 0.9982, recoveries between 94.0 and 102.4%, and reproducibility with RSD lower than 4.5%. The method was applied to simultaneously determine the compounds in 60 different beverage samples, including beer, coffee, black tea, and fruit juices. The presence of secondary lipid oxidation products is demonstrated in beverages with a strong roasting process or oxidation.
一种新的、快速、简单、有效的超声辅助分散液液微萃取程序（UA-DLLME）已成功开发，用于气相色谱-质谱（GC-MS）测定饮料中的丙二醛、丙烯醛和 4-羟基-2-壬烯醛。萃取过程中进行了 2,4-二硝基苯肼衍生化。采用不对称 34//18 筛选设计和中心复合表面响应设计来研究萃取过程中最关键因素（超声时间和温度、萃取和分散溶剂体积、盐添加量和衍生化试剂浓度）的影响。根据 FDA 指南对该方法进行了验证，实现了良好的线性度，r≥0.9982，回收率在 94.0%至 102.4%之间，重现性 RSD 低于 4.5%。该方法应用于同时测定 60 种不同饮料样品中的化合物，包括啤酒、咖啡、红茶和果汁。在具有强烈烘焙过程或氧化的饮料中证明存在次级脂质氧化产物。
