Green infant formula analysis: Optimizing headspace solid-phase microextraction of carbonyl compounds associated with lipid peroxidation using GC-MS and pentafluorophenylhydrazine derivatization.

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.

Determination of synthetic opioids in oral fluid samples using fabric phase sorptive extraction and gas chromatography-mass spectrometry.

New psychoactive substances (NPS) continue to emerge in the drug market every year, becoming a global threat to public health and safety. These compounds are mostly synthetic cannabinoids and designer cathinones. However, synthetic opioids have appeared on the recreational drug markets in recent years, particularly fentanyl and its derivatives ("fentanyls"). Fentanyl and its analogs are related to harmful intoxications and an increase in opioid-related mortality in many countries, such as in the United States and Europe in the last years. Taking the drug related global crisis into consideration, this work developed and validated an effective and sensitive method based on fabric phase sorptive extraction (FPSE) followed by gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of 11 fentanyl analogs in oral fluid samples. The extraction was carried out using a sol-gel Carbowax 20 M sorbent immobilized on 100% cellulose fabric substrate and using ethyl acetate as the desorption solvent. The limits of detection (LODs) and quantification (LOQs) ranged from 1 to 15 ng mL-1 and 5 to 50 ng mL-1, respectively. Intra-day and inter-day precision were found within 8.2% and 8.6%, respectively, while accuracy ranged from -5.5 to 9.1%, in accordance with the established criteria. The absolute recovery values were in the range of 94.5%-109.1%. The validated method demonstrated its great potential to detect and quantify fentanyl analogs in possible forensic work and off-site analysis in road traffic cases.