ACE is categorized as possibly carcinogenic to humans (Group 2B), suggesting it may be carcinogenic, with an Acceptable Daily Intake (ADI) of 185 \(\upmu\)g/day. MDA falls into the group of substances with insufficient evidence for their carcinogenicity (Group 3). However, it possesses a Threshold of Toxicological Concern set by the International Programme on Chemical Safety (IPCS) of 30 \(\upmu\)g/kg bw/day. MGO is also in Group 3 and does not have a specific TDI. Finally, while unclassified by the IARC, DA has a notable ADI of 900 \(\upmu\)g/kg bw/day [7; 8; 9; 10; 11; 12]. Given the potential health implications of these contaminants, the need for reliable analytical methods to assess their levels in adult formulas is paramount [7]. Traditional methods for determining lipid peroxidation products in foods, such as the thiobarbituric acid (TBA) test and peroxide value measurement, are widely used due to their simplicity and accessibility [7; 13; 14]. However, these methods have several limitations: they are non-specific (which can lead to overestimation), time-consuming, and require harsh conditions and large amounts of solvents, which have a notable environmental impact [13; 14]. To address these limitations, chromatographic methods such as high-performance liquid chromatography (HPLC) and gas chromatography (GC), paired with various detection systems (UV, Fluorescence Detection (FLD), Flame Ionization Detection (FID), and Mass Spectrometry (MS)), have been developed [7; 13; 14; 15; 16; 17; 18; 19; 20]. These methods allow for the specific determination of lipid peroxidation products, including aldehydes, ketones, malondialdehydehyde, and dicarbonyl compounds, with higher sensitivity and selectivity than traditional methods [7]. However, to detect specific compounds like AGEs and other lipid peroxidation products effectively, chemical derivatization (e.g., with hydrazine, TBA, or o-phenylene diamine) is often required to enhance instrument response, depending on the detector system [13; 17; 18; 19; 20]. Microextraction techniques have further advanced the sensitivity and specificity of carbonyl compounds and VOCs analysis by offering a more sustainable approach due to the reduced sample size and waste generation and the reduction (Dispersive Liquid-Liquid Microextraction, DLLME) or non-use (Solid Phase Microextraction, SPME) of organic solvent [7]. In this context, head-space (HS) SPME has been used to determine carbonyl compounds associated with lipid peroxidation in infant formula, milk, and dairy products [7; 20; 21]. VOC determination without derivatization has also been reported usingHS-SPME [7]. DLLME has been applied to measure FCHO, MDA, and ACRL [7; 16; 22] in beverages. To our knowledge, there is no analytical method for assessing lipid peroxidation products in adult formula products. In this study, we aim to apply innovative microextraction techniques to determine the concentrations of carbonyl compounds and to monitor VOCs in adult formulas. Specifically, we propose using DLLME for the targeted analysis of carbonyl and dicarbonyl compounds as potential markers of lipid peroxidation and HS-SPME for untargeted VOC determination, as it requires no derivatization. Through these methods, we present the first known data on the occurrence of carbonyl compounds associated with oxidative and storage stability in adult formulas, as far as we know. Additionally, we assess the potential risk of exposure for consumers to these contaminants, highlighting the need for ongoing monitoring to warrant the safety and quality of adult formula.