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


Vazquez L. Celeiro M. Sergazina M. Dagnac T. Llompart M.
June 2021Elsevier B.V.

Sustainable Chemistry and Pharmacy
2021#21

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 suitability.

Experimental design , GC-MS , Honey , Miniaturized solid phase microextraction

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CRETUS Institute, Department of Analytical Chemistry, Nutrition and Food Science, Universidade de Santiago de Compostela, Santiago de Compostela, E-15782, Spain
Department of Chemistry, Institute of Natural Science and Geography, Abai Kazakh National Pedagogical University, Almaty, Kazakhstan
Galician Agency for Food Quality - Agronomic Research Centre (AGACAL-CIAM) – Unit of Organic Contaminants, Apartado 10, A Coruña, E-15080, Spain

CRETUS Institute
Department of Chemistry
Galician Agency for Food Quality - Agronomic Research Centre (AGACAL-CIAM) – Unit of Organic Contaminants

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