RT Journal Article
T1 Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts
A1 Rangel Silva, Alexandra
A1 Custodio Mendoza, Jorge Antonio
A1 Rodrigo Santos, João
A1 Almeida, Paulo Jorge Silva
A1 Rodrigues, José António Maia
A1 Carro Díaz, Antonia María
K1 Carbonyl compounds
K1 Coffee
K1 Dispersive liquid-liquid microextraction
K1 GC-MS
K1 Low-density extractant solvent
K1 Sample preparation
AB This work presents a greener approach for ultrasound-assisted (UA) dispersive liquid-liquid microextraction (DLLME) of carbonyl compounds from coffee samples, before GC–MS determination. This work aims to substitute the solvents used in the traditional DLLME procedures with greener alternatives and to decrease the volume of solvents used. Low-density solvents, 1-octanol and isooctane, were evaluated as the extraction solvent. Optimization of critical experimental parameters was conducted in two stages: an asymmetrical screening design 2331 // 8, followed by a Doehlert experimental design. In the first experimental design 4 parameters were optimized: the volume of aqueous phase volume (1.5 mL), the concentration of the derivatization reagent solution pentafluorophenylhydrazine (1.12 g/L) and the volume and type of extraction solvent (60 µL of isooctane). In the second experimental design, 15 min of derivatization at 50 °C were selected as optimized conditions. The enrichment factor associated with the DLLME procedure enabled the efficient extraction of nine carbonyl compounds (acetaldehyde, acrolein, benzaldehyde, diacetyl, formaldehyde, furfural, glyoxal, malondialdehyde, and methylglyoxal) from coffee samples. The method demonstrated strong analytical performance, with figures of merit including r2 ≥ 0.9990, limits of detection between 289 and 436 µg/L, intraday, and interday precisions < 9.5 %. Recovery values for all nine carbonyl compounds ranged from 90.0 to 110.0 %. The greenness of the developed methodology was assessed using the AGREEprep tool, yielding a score of 0.59. Acetaldehyde, benzaldehyde and furfural were quantified in most coffee samples analyzed, with no significant differences observed in carbonyl compounds composition.
PB Elsevier
SN 0021-9673
YR 2025
FD 2025-03-29
LK https://hdl.handle.net/10347/43302
UL https://hdl.handle.net/10347/43302
LA eng
NO References  Silva, A. R., Custodio-Mendonza, J. A., Santos, J. R., Almeida, P. J., Rodrigues, J. A., & Carro, A. M. (2025). Green solvents in dispersive liquid-liquid microextraction for the determination of carbonyl compounds in coffee extracts. Journal of Chromatography A, 1745, 465743. 10.1016/j.chroma.2025.465743
NO This work was supported by the Portuguese government through The Foundation for Science and Technology (FCT/MCTES) under the project UIDP/50006/2020 (DOI 10.54499/UIDP/50006/2020) and national funds. And also received support from Polish National Science Center within the project 2023/07/X/NZ9/01113 as part of the MINIATURA-7 program.
NO This work received financial support from PT national funds (FCT/ MCTES, Fundaç˜ ao para a Ciˆencia e Tecnologia and Minist´erio da Ciˆencia, Tecnologia e Ensino Superior) through the projects UIDB/50006/ 2020 and UIDP/50006/2020. ARS acknowledges her PhD grant (ref. 2021.05227.BD) supported by FCT. J.R. Santos acknowledges the program DL 57/2016 – Norma transitoria ´ (ref. SFRH/BPD/76544/2011 respectively) supported by FCT. The article is based upon work from the Sample Preparation Study Group and Network, supported by the Division of Analytical Chemistry of the European Chemical Society.
DS Minerva
RD 24 abr 2026