Optimization of a miniaturized solid-phase microextraction method followed by gas chromatography mass spectrometry for the determination of twenty four volatile and semivolatile compounds in honey from Galicia (NW Spain) and foreign countries

An analytical miniaturized methodology based on solid-phase-microextraction (mini_SPME) followed by gas chromatography coupled to mass spectrometry (GC-MS) has been developed for the identification of volatile and semivolatile compounds in honey samples. The main influential experimental parameters, such as the type of fibre coating, extraction temperature, solvent addition, extraction mode, ionic strength, and sample dilution were optimized. A design of experiments (DOE) was conducted including twenty-four target compounds. The final extraction conditions comprised the use of 200 mg of honey mixed with 200 μL of water (100%, w/v), employing a DVB/CAR/PDMS fibre in the headspace mode at 100 °C for 30 min. The mini_SPME-GC-MS method was successfully validated in terms of linearity, repeatability, reproducibility and accuracy. Finally, it was applied to a broad range of varieties of real honey samples from Galicia (NW Spain), as well as some foreign honeys, demonstrating suitabilityThis research was supported by GO project FEADER 2018/054B. The authors belong to the National Network for the Innovation in miniaturized sample preparation techniques, RED2018-102522-T (Ministry of Science, Innovation and Universities, Spain), to the Galician Competitive Research Groups IN607B 2019/13 and ED431 2020/06 and to the CRETUS Strategic Partnership ED431 2018/01 (Xunta de Galicia)S