Multi-target optimization of solid phase microextraction to analyse key flavour compounds in wort and beer.

Despite the literature comprises numerous studies dealing with the analysis of wort and beer flavour-related compounds by HS-SPME followed by GC-MS quantification, no generalized consensus exists regarding the optimal conditions for the extraction procedure. The complex chemistry nature of these matrices, the number of analytes, as well as the number and interactions among parameters affecting the extraction performance, requires the adoption of optimal experimental design protocols. This aspect is often overlooked and often not properly addressed in practice. Therefore, in the present work, the optimal conditions under which a range of wort and beer analytes can be extracted and quantified were analysed. The optimal extraction conditions were presented at two levels of aggregation: global (untargeted) and key-flavour analysis. Experimental data was generated by Definitive-Screening-Design, followed by model development and optimization. Both approaches were compared and critically analysed. For vicinal-diketones group, a complete validation study for the optimal conditions is presented.

[1]  Victor R. Preedy,et al.  Beer in health and disease prevention , 2009 .

[2]  Henryk H. Jeleń,et al.  Solid-Phase Microextraction for the Analysis of Some Alcohols and Esters in Beer: Comparison with Static Headspace Method , 1998 .

[3]  Fengshan Bai,et al.  Constructing Definitive Screening Designs Using Conference Matrices , 2012 .

[4]  Christopher J. Nachtsheim,et al.  Definitive Screening Designs with Added Two-Level Categorical Factors* , 2013 .

[5]  T. Brandão,et al.  Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers. , 2013, Talanta.

[6]  S. Rocha,et al.  Insights on beer volatile profile: Optimization of solid-phase microextraction procedure taking advantage of the comprehensive two-dimensional gas chromatography structured separation. , 2015, Journal of Separation Science.

[7]  S. Buxaderas,et al.  Assessment of the aroma profiles of low-alcohol beers using HS-SPME–GC-MS , 2014 .

[8]  D. Saison,et al.  Decrease of 4-vinylguaiacol during beer aging and formation of apocynol and vanillin in beer. , 2008, Journal of agricultural and food chemistry.

[9]  Jean-François Focant,et al.  Advanced method optimization for volatile aroma profiling of beer using two-dimensional gas chromatography time-of-flight mass spectrometry. , 2017, Journal of chromatography. A.

[10]  Paul S. Hughes,et al.  Beer: Quality, Safety and Nutritional Aspects , 2001 .

[11]  T. Fushiki,et al.  Testing for Taste and Flavour of Beer , 2002 .

[12]  I. Márová,et al.  Determination of trans-2-nonenal in barley grain, malt and beer , 2010 .

[13]  Ana C. Pereira,et al.  Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection. , 2015, Analytica chimica acta.

[14]  D. Saison,et al.  Optimisation of a complete method for the analysis of volatiles involved in the flavour stability of beer by solid-phase microextraction in combination with gas chromatography and mass spectrometry. , 2008, Journal of chromatography. A.

[15]  J. S. Hough,et al.  Malting and brewing science , 1971 .

[16]  P. Veselý,et al.  Analysis of aldehydes in beer using solid-phase microextraction with on-fiber derivatization and gas chromatography/mass spectrometry. , 2003, Journal of agricultural and food chemistry.

[17]  K. Verstrepen,et al.  Production and biological function of volatile esters in Saccharomyces cerevisiae , 2010, Microbial biotechnology.

[18]  L. Huimin,et al.  Analysis of volatile flavor compounds in top fermented wheat beer by headspace sampling-gas chromatography , 2012 .

[19]  V. Kellner,et al.  Analysis of Selected Esters in Beer: Comparison of Solid-Phase Microextraction and Stir Bar Sorptive Extraction , 2010 .

[20]  Jânio Sousa Santos,et al.  Use of principal component analysis (PCA) and hierarchical cluster analysis (HCA) for multivariate association between bioactive compounds and functional properties in foods: A critical perspective , 2018 .

[21]  S. Ebeler,et al.  Headspace solid-phase microextraction for the analysis of dimethyl sulfide in beer. , 1999, Journal of Agricultural and Food Chemistry.

[22]  Fabio Augusto,et al.  Exploratory analysis of the volatile profile of beers by HS–SPME–GC , 2008 .

[23]  G. Moris,et al.  Quantification of Six Phthalates and One Adipate in Luxembourgish Beer Using HS-SPME-GC/MS , 2017, Food Analytical Methods.

[24]  R. Raices,et al.  Method development by GC-ECD and HS-SPME-GC-MS for beer volatile analysis. , 2015, Food chemistry.

[25]  D. Saison,et al.  Optimisation of wort volatile analysis by headspace solid-phase microextraction in combination with gas chromatography and mass spectrometry. , 2008, Journal of chromatography. A.

[26]  A. Olaniran,et al.  Aroma-active ester profile of ale beer produced under different fermentation and nutritional conditions. , 2014, Journal of bioscience and bioengineering.

[27]  P. Silcock,et al.  Comparison of four extraction methods for analysis of volatile hop-derived aroma compounds in beer. , 2017, Journal of separation science.

[28]  R. Wagner,et al.  (E)-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS) , 2010 .

[29]  G. Perretti,et al.  Characterization of the volatile profiles of beer using headspace solid-phase microextraction and gas chromatography-mass spectrometry. , 2014, Journal of the science of food and agriculture.

[30]  C. Muñoz-González,et al.  Optimization of a HS-SPME-GC-MS Procedure for Beer Volatile Profiling Using Response Surface Methodology: Application to Follow Aroma Stability of Beers Under Different Storage Conditions , 2012, Food Analytical Methods.

[31]  C. Blanco,et al.  New trends in beer flavour compound analysis. , 2015, Journal of the science of food and agriculture.

[32]  Doehlert design-desirability function multi-criteria optimal separation of 17 phenolic compounds from extra-virgin olive oil by capillary zone electrophoresis. , 2014, Food chemistry.

[33]  David E. Quain,et al.  Brewing Yeast and Fermentation , 2001 .

[34]  P. Dostálek,et al.  Application of response surface design to optimise the chromatographic analysis of volatile compounds in beer , 2018, Journal of the Institute of Brewing.

[35]  M. Gastl,et al.  Processing of a Top Fermented Beer Brewed from 100% Buckwheat Malt with Sensory and Analytical Characterisation , 2010 .

[36]  F. J. Pérez,et al.  Beer volatile analysis: optimization of HS/SPME coupled to GC/MS/FID. , 2011, Journal of food science.

[37]  S. Kang,et al.  Influence of aeration during propagation of pitching yeast on fermentation and beer flavor. , 2007, Journal of microbiology and biotechnology.

[38]  A. Olaniran,et al.  Stability profile of flavour-active ester compounds in ale and lager beer during storage , 2013 .

[39]  Marco S. Reis,et al.  Definitive Screening Designs and latent variable modelling for the optimization of solid phase microextraction (SPME): Case study - Quantification of volatile fatty acids in wines , 2018, Chemometrics and Intelligent Laboratory Systems.

[40]  C. Pizarro,et al.  Optimisation of a simple and reliable method based on headspace solid-phase microextraction for the determination of volatile phenols in beer. , 2010, Journal of chromatography. A.

[41]  Xiaolan Chai,et al.  Study of Chromatographic Fingerprint of the Flavor in Beer by HS-SPME-GC , 2011 .

[42]  Jessika De Clippeleer,et al.  Flavour Instability of Pale Lager Beers: Determination of Analytical Markers in Relation to Sensory Ageing , 2008 .

[43]  Christopher J. Nachtsheim,et al.  A Class of Three-Level Designs for Definitive Screening in the Presence of Second-Order Effects , 2011 .

[44]  F. Rodrigues,et al.  Development of a dynamic headspace solid-phase microextraction procedure coupled to GC-qMSD for evaluation the chemical profile in alcoholic beverages. , 2008, Analytica chimica acta.

[45]  Sergio L C Ferreira,et al.  Multivariate optimization techniques in food analysis - A review. , 2017, Food chemistry.

[46]  R. Smith,et al.  Determination of sulphur compounds in beer using headspace solid-phase microextraction and gas chromatographic analysis with pulsed flame photometric detection. , 2000, Journal of chromatography. A.

[47]  Jana Hajslova,et al.  Recognition of beer brand based on multivariate analysis of volatile fingerprint. , 2010, Journal of chromatography. A.

[48]  G. Li,et al.  Quantitative Analysis of Flavor Volatiles in Beer Using Headspace Solid-Phase Microextraction and Gas Chromatography–Flame Ionization Detection (HS-SPME-GC-FID) , 2015 .

[49]  K. Krogerus,et al.  Influence of valine and other amino acids on total diacetyl and 2,3-pentanedione levels during fermentation of brewer’s wort , 2013, Applied Microbiology and Biotechnology.

[50]  F. Marini,et al.  Flavour component analysis by HS-SPME/GC–MS and chemometric modeling to characterize Pilsner-style Lager craft beers , 2019, Microchemical Journal.

[51]  Relationships of Overall Estery Aroma Character in Lagers with Volatile Headspace Congener Concentrations , 2006 .

[52]  J. Teixeira,et al.  A review of flavour formation in continuous beer fermentations , 2008 .

[53]  C. L. Biazon,et al.  Combining silica-based adsorbents and SPME fibers in the extraction of the volatiles of beer: an exploratory study , 2009, Analytical and bioanalytical chemistry.

[54]  Marcos Almeida Bezerra,et al.  Simplex optimization: A tutorial approach and recent applications in analytical chemistry , 2016 .

[55]  F. Gomes,et al.  Identification of volatile organic compounds extracted by headspace solid‐phase microextraction in specialty beers produced in Brazil , 2017 .

[56]  E. Busto,et al.  Analysis of beer volatiles by polymeric imidazolium-solid phase microextraction coatings: Synthesis and characterization of polymeric imidazolium ionic liquids. , 2013, Journal of chromatography. A.

[57]  I. Márová,et al.  Optimization of Modern Analytical SPME and SPDE Methods for Determination of Trans-2-nonenal in Barley, Malt and Beer , 2011 .

[58]  H. Suomalainen,et al.  Aroma of Beer, Wine and Distilled Alcoholic Beverages , 1983 .

[59]  H. Goicoechea,et al.  Experimental design and multiple response optimization. Using the desirability function in analytical methods development. , 2014, Talanta.

[60]  Daniel Granato,et al.  Classification of juices and fermented beverages made from unripe, ripe and senescent apples based on the aromatic profile using chemometrics. , 2013, Food chemistry.

[61]  I. Ferreira,et al.  Method optimization by solid-phase microextraction in combination with gas chromatography with mass spectrometry for analysis of beer volatile fraction. , 2006, Journal of chromatography. A.

[62]  F. Delvaux,et al.  Determination of hydroxycinnamic acids and volatile phenols in wort and beer by isocratic high-performance liquid chromatography using electrochemical detection. , 2006, Journal of chromatography. A.

[63]  J. Mareček,et al.  Monitoring Volatile Substances in Beer in Relation to Beer Production Technology , 2015 .