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Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection
Advisor(s)
Abstract(s)
Vicinal diketones, namely diacetyl (DC) and pentanedione (PN), are compounds naturally found in beer
that play a key role in the definition of its aroma. In lager beer, they are responsible for off-flavors
(buttery flavor) and therefore their presence and quantification is of paramount importance to beer
producers. Aiming at developing an accurate quantitative monitoring scheme to follow these off-flavor
compounds during beer production and in the final product, the head space solid-phase microextraction
(HS-SPME) analytical procedure was tuned through experiments planned in an optimal way and the final
settings were fully validated. Optimal design of experiments (O-DOE) is a computational, statistically oriented approach for designing experiences that are most informative according to a well-defined
criterion. This methodology was applied for HS-SPME optimization, leading to the following optimal
extraction conditions for the quantification of VDK: use a CAR/PDMS fiber, 5 ml of samples in 20 ml vial,
5 min of pre-incubation time followed by 25 min of extraction at 30 C, with agitation. The validation of
the final analytical methodology was performed using a matrix-matched calibration, in order to mini mize matrix effects. The following key features were obtained: linearity (R2 > 0.999, both for diacetyl and
2,3-pentanedione), high sensitivity (LOD of 0.92 mg L 1 and 2.80 mg L 1
, and LOQ of 3.30 mg L 1 and
10.01 mg L 1
, for diacetyl and 2,3-pentanedione, respectively), recoveries of approximately 100% and
suitable precision (repeatability and reproducibility lower than 3% and 7.5%, respectively). The applicability of the methodology was fully confirmed through an independent analysis of several beer
samples, with analyte concentrations ranging from 4 to 200 g L 1
Description
Keywords
Vicinal diketones Headspace solid phase microextraction Optimization Optimal design of experiments . Faculdade de Ciências da Vida Escola Superior de Tecnologias e Gestão Faculdade de Ciências Exatas e da Engenharia
Citation
Leça, J. M., Pereira, A. C., Vieira, A. C., Reis, M. S., & Marques, J. C. (2015). Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection. Analytica chimica acta, 887, 101-110. https://doi.org/10.1016/j.aca.2015.06.044
Publisher
Elsevier