RT Journal Article
T1 Green infant formula analysis: Optimizing headspace solid-phase microextraction of carbonyl compounds associated with lipid peroxidation using GC-MS and pentafluorophenylhydrazine derivatization
A1 Custodio Mendoza, Jorge Antonio
A1 López Blanco, Ana
A1 Ares-Fuentes, Ana María
A1 Carro Díaz, Antonia María
K1 GC-MS
K1 Glyoxal
K1 HS-SPME
K1 Infant formula
K1 Malondialdehyde
K1 Methylglyoxal
AB The refinement and optimization of a method combining headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was successfully performed for the first time to determine seven carbonyl and dicarbonyl compounds, including glyoxal, methylglyoxal, dimethylglyoxal, and malondialdehyde in infant formulae, related to lipid peroxidation. HS-SPME was utilized for simultaneous extraction and derivatization with pentafluorophenylhydrazine (PFPH). Critical parameters such as temperature, pH, extractive phase, and salting-out were meticulously investigated and fine-tuned by an asymmetrical 2232//9 screening design to ensure the method's efficacy and reliability. Optimal conditions included a PFPH concentration of 5 g/L, pH 5.0, head-space extraction at 60 °C within 10 min, utilizing a DVB/CAR/PDMS coating, and a 20% w/w salting-out. The analytical validation of this method, compliant with FDA guidelines, demonstrated exceptional linearity, sensitivity, specificity, precision (RSD ≤13.8%), and accuracy (84.8% ≤ recovery ≤111.5%). The metric approach AGREEprep confirms its eco-friendliness, marking a significant step towards an environmentally conscious approach in infant formula analysis. An occurrence study conducted on 25 infant formula samples revealed widespread carbonyl and dicarbonyl compounds in both powdered and liquid variants. ANOVA results exhibited variations in compound concentrations among different sample groups. Clustering analyses delineated distinct groups based on carbonyl content, indicating the potential of these compounds as markers for lipid peroxidation and food quality assessment. This method serves as a valuable tool for evaluating infant formula quality, stability towards oxidation, and safety.
PB Elsevier
SN 0039-9140
YR 2024
FD 2024
LK http://hdl.handle.net/10347/33829
UL http://hdl.handle.net/10347/33829
LA eng
NO Talanta Volume 273, 1 June 2024, 125816
NO This work was supported by the Spanish Ministry of Science, Innovation, and Universities (Project RTI2018‐096450‐B‐I00) along with FEDER founds, and by the Polish National Science Centre (Project 2023/07/X/NZ9/01113) as part of the MINIATURA-7 program.
DS Minerva
RD 27 abr 2026