4.7 Article

Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection

期刊

ANALYTICA CHIMICA ACTA
卷 887, 期 -, 页码 101-110

出版社

ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2015.06.044

关键词

Vicinal diketones; Headspace solid phase microextraction; Optimization; Optimal design of experiments

资金

  1. Agencia Regional para o Desenvolvimento da Investigacao Tecnologia e Inovacao (ARDITI) [0002376/2014/131, 002248/2013/131]
  2. FEDER [MADFDR-01-0224-FEDER-000006]

向作者/读者索取更多资源

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 degrees C, with agitation. The validation of the final analytical methodology was performed using a matrix-matched calibration, in order to minimize matrix effects. The following key features were obtained: linearity (R-2 > 0.999, both for diacetyl and 2,3-pentanedione), high sensitivity (LOD of 0.92 mu g L-1 and 2.80 mu g L-1, and LOQ of 3.30 mu g L-1 and 10.01 mu g 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. (C) 2015 Elsevier B.V. All rights reserved.

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