Development of a fiber derivatization method for the analysis of 18 carbonyl compounds in roasted lamb using HS-SPME/GC-TQ/MS

A method based on headspace solid-phase microextraction fiber derivatization (HS-SPME-FD) coupled with gas chromatography-triple quadrupole mass spectrometry (GC-TQ/MS) was developed to quantify 18 flavor-related carbonyl compounds in roasted lamb. Optimization of derivatization conditions established the following optimal parameters: a 3 g/L concentration of O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), fiber loading at 50 °C for 5 min, followed by simultaneous extraction/derivatization at 50 °C for 30 min. The method was validated for linearity, limits of detection (LOD), limits of quantification (LOQ), precision, and accuracy. Results confirmed the method's suitability for determining carbonyl compounds in roasted lamb. During roasting, the composition and concentration of carbonyl compounds increased significantly, with hexanal being the most abundant. Additionally, the method detected carbonyl compounds in the model system at levels comparable to real roasted lamb, validating both the model's accuracy and the method's quantitative precision.