Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry using isotope dilution

• Published in: Journal of Chromatography A 2003-10, Vol.1017 (1), p.141-149
• Main Authors: Giordano, Lucia, Calabrese, Roberto, Davoli, Enrico, Rotilio, Domenico
• Format: Article
• Language: English
• Subjects: 5-Methylfurfural; Acetic Acid - chemistry; Biological and medical sciences; Calibration; Fermented food industries; Food analysis; Food industries; Fundamental and applied biological sciences. Psychology; Furaldehyde - analogs & derivatives; Furaldehyde - analysis; Furfurals; Gas Chromatography-Mass Spectrometry - methods; Isotopes; Isotopic dilution; Salts; Temperature; Vinegar; Wines and vinegars
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2003.08.029

A new method was developed for the determination of 2-furfural (2-F) and 5-methylfurfural (5-MF), two products of Maillard reaction in vinegar, with head-space solid-phase microextraction (HS-SPME) coupled to gas chromatography–mass spectrometry (GC–MS). A divinylbenzene (DVB)/carboxen (CAR)/polydimethylsiloxane (PDMS) fibre was used and SPME conditions were optimised, studying ionic strength effect, temperature effect and adsorption time. Both analytes were determined by calibration established on 2-furfural-d 4 (2-F-d 4). The method showed good linearity in the range studied (from 16 to 0.12 mg/l), with a regression coefficient r 2 of 0.9999. Inter-batch precision and accuracy were found between 14.9 and 6.0% and between −11.7 and 0.2%, respectively. Detection limit was 15 μg/l. The method is simple and accurate and it has been applied to a series of balsamic and non-balsamic vinegars.