RT Journal Article T1 GC–MS determination of malondialdehyde, acrolein, and 4-hydroxy-2-nonenal by ultrasound-assisted dispersive liquid-liquid microextraction in beverages A1 Custodio Mendoza, Jorge A1 Caamaño Fernández, Cristian A1 Lage Yusti, María Asunción A1 Almeida, Paulo Joaquim Ferreira de A1 Lorenzo, Rosa Antonia A1 Carro Díaz, Antonia María K1 4-hydroxy-2-nonenal K1 Acrolein K1 Malondialdehyde K1 Dispersive liquid-liquid microextraction K1 Beverages AB 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 3541//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 r2 ≥ 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 PB Elsevier YR 2022 FD 2022 LK http://hdl.handle.net/10347/29035 UL http://hdl.handle.net/10347/29035 LA eng NO Food Chemistry 384 (2022) 132530 NO This work was supported by the Spanish Ministry of Science, Innovation, and Universities (Project RTI2018‐096450‐B‐I00) and FEDER funds DS Minerva RD 22 abr 2026