Citrus sinensis (orange) by-products represent one of the most abundant citric residues from orange juice industrial production, and are a promising source of health-promoting compounds like terpenes.

This work presents a headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for the analysis of solid food samples in extended experiments. The final procedure was used to quantify 30 volatile compounds in fresh beef. The strategy adds robustness to the classic SPME methods for solid samples, by including a control solution that solves several challenges. The control solution contained one representative compound for each studied family of beef, and two internal standards. Response factors were calculated for each family, and were subsequently applied to every compound belonging to the same family. This strategy allowed control of the quantification procedure even when the fibre, column or control solution changed. Repeatability and reproducibility had relative standard deviation values below 17%, except for phenylacetaldehyde, (E)-2-nonenal and (E,Z)-2,4-decadienal. Although the method described here was applied to animal products, it has also been successfully used to distinguish between samples from different lipid oxidation stabilities.