Green Ultrasound-Assisted Dispersive Liquid–Liquid Microextraction Coupled to GC–MS for Simultaneous Determination of Lipid-Peroxidation- and Maillard-Derived Carbonyl Compounds in Plant-Based Beverages

Carbonyl compounds generated through lipid peroxidation and Maillard-type reactions are relevant markers of food quality and safety due to their potential toxicity and prevalence in processed plant-based beverages. This work presents the development and validation of a green, ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) method using sustainable extractant (isobutyl acetate) and dispersant (isopropanol) solvents for the simultaneous determination of 12 carbonyl compounds across multiple chemical families (aldehydes, ketones, furans, and dicarbonyls). The method integrates in situ derivatization with <i>O</i>-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride and gas chromatography-mass spectrometry (GC-MS) analysis. Method optimization was performed using a multivariable approach using an asymmetrical 2⁶·3¹ screening design and a central composite design for response surface methodology. Analytical performance was validated according to Food and Drug Administration guidelines, achieving great linearity (<i>r</i> ² ≥ 0.9991), accuracy (90-107% recovery), precision (<7.5% RSD) and detection limits suitable for trace-level analysis in complex matrixes. The approach was applied to 51 commercial plant-based beverage samples (almond, soy, oat, rice, coconut, seed and mixed formulations). Greenness assessment was performed using AGREEprep (0.69/1) and BAGI (77.5/100) metrics, confirming the method's alignment with green chemistry principles. This workflow provides a reliable and sustainable strategy for routine monitoring of carbonyls in food systems, with relevance to both quality control and exposure assessment.