LWT - Food Science and Technology 191 (2024) 115662

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LWT
journal homepage: www.elsevier.com/locate/lwt

Effects of progressive freeze concentration on craft beer: Volatile

compounds, sensory profile, and physicochemical characteristics
M. Osorio a, b, F.L. Moreno b, E. Hernández c, Annamaria Filomena-Ambrosio b, d, Coralia Osorio e,
Y. Ruiz b, *
a
Doctoral Program in Engineering, Faculty of Engineering, Universidad de La Sabana, Chia, Colombia
b
Grupo de Investigación en Procesos Agroindustriales, Universidad de La Sabana, Chía, Colombia
c
Agri-Food Engineering and Biotechnology Department, Universidad Politécnica de Cataluña (UPC),Castelldefels, Barcelona, Spain
d
Research group in Alimentación, Gestión de Procesos y Servicio, EICEA, Universidad de La Sabana, Chía, Colombia
e
Departamento de Química, Universidad Nacional de Colombia, Bogotá, 14490, Colombia

A R T I C L E I N F O A B S T R A C T

Keywords: Craft beers are becoming increasingly popular due to their developed and complex flavours, and there is a po­
Craft beer tential market for developing concentrated products; thus, freeze concentration can exploit this opportunity. In
Freeze concentration this work, the changes in physicochemical properties, volatile organic compounds, and sensory profiles of three
Volatile compounds
craft beers (Witbier, Bitter, and Porter) after applying progressive stirred freeze concentration (PSFC) were
Sensory profile
evaluated, both on the concentrated liquid fraction and the ice fraction. After freeze concentration, increasing the
concentration of all physicochemical characteristics in the three beers was possible. It was also possible to
preserve the distribution of the volatile components in the liquid fractions and change it in the ice fractions.
Significant differences were found in the sensory analysis of the concentrated liquid and the recovered ice
fractions, and they were associated with the changes in the volatiles and the physicochemical properties. PSFC
presents an opportunity to develop new beer products since both fractions show the potential to be
commercialized.

1. Introduction
Beer is a complex product with five major components and over 800
organic compounds from the raw materials, the brewing process or
storage, as shown in Fig. 1 (Buiatti, 2008; Verhagen, 2010). Some of
these compounds are nonvolatile compounds, such as polyphenols or
hops alfa-acids (Bertuzzi et al., 2020; D. O. Carvalho & Guido, 2022;
Cortese et al., 2020; Gonzalez Viejo, Fuentes, Torrico, Godbole, &
Dunshea, 2019; Sohrabvandi, Mortazavian, & Rezaei, 2012; Verhagen,
2010), and others are volatile compounds, such as alcohols, aldehydes,
and furans (Alves et al., 2020; Coelho et al., 2019; Verhagen, 2010).
Overall, the interaction of all these compounds affects the flavour, giv­
ing each brew distinctive profile (Alves et al., 2020).
Beer can be divided into two categories: industrial beer, usually
brewed by bottom fermentation (Lager type), and craft beer, tradition­
ally produced by top fermentation (Ale type) (Fang et al., 2022; Pal­
mioli, Alberici, Ciaramelli, & Airoldi, 2020). The growing demand for
diversity, quality, and sensory complexity, named the “flavour
revolution”, has opened an opportunity for craft ale beers worldwide
(Aquilani, Laureti, Poponi, & Secondi, 2015; Callejo, Tesfaye, & Morata,
2020; Gómez-Corona, Escalona-Buendía, García, Chollet, & Valentin,
2016) because they have more developed and complex flavours than the
Lager type (Tang & Li, 2017). The industry of craft beer continues to
expand because its consumers look for novel and complex flavour pro­
files, which creates an opportunity for diversification of beer styles,
flavour qualities, and intensities and the development of new products
based on new technologies and ideas (Jaeger, Worch, Phelps, Jin, &
Cardello, 2020; Tang & Li, 2017; Villacreces, Blanco, & Caballero,
2022). It is possible to modify the concentration of the compounds
responsible for flavour, thus generating concentrated beer products,
highlighting the attributes consumers value most (Miyawaki et al., 2016;
Osorio, Moreno, Hernández, & Ruiz-Pardo, 2023; Wu et al., 2017).
Therefore, it is necessary to use a technique that allows the removal
of water, avoiding the impact of compounds sensitive to temperature or
the loss of volatiles, such as freeze concentration (FC), which is a method
based on removing water from a solution by cooling and freezing until

* Corresponding author.
E-mail address: ruth.ruiz@unisabana.edu.co (Y. Ruiz).

https://doi.org/10.1016/j.lwt.2023.115662
Received 25 August 2023; Received in revised form 6 December 2023; Accepted 13 December 2023
Available online 17 December 2023
0023-6438/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).
M. Osorio et al.
high purity ice crystals are formed and separated (Miyawaki & Inakuma,
2021). FC has shown promising results regarding the concentrations
achieved and the preservation or enhancement of organoleptic proper­
ties and bioactivity (Almeida et al., 2023; Barros et al., 2021; Haas et al.,
2022; Moreno et al., 2015; Orellana-Palma, Petzold, Pierre, & Pensaben,
2017; Orellana-Palma, Tobar-Bolaños, Casas-Forero, Zúñiga, & Petzold,
2020; Samsuri, Li, Ruslan, & Amran, 2020). Several FC techniques are
grouped into three categories: suspension, layer, and block (Miyawaki &
Inakuma, 2021). Suspension FC is a high-performance process but in­
volves high investments and operation costs (Sánchez, Ruiz, Auleda,
Hernandez, & Raventos, 2009). Therefore, improving other more
affordable techniques, such as progressive FC, is essential. For example,
the progressive stirred freeze concentration (PSFC) quickly achieves a
high concentration index, although it may have ice layer occlusion
(Masuda, Ryuzaki, & Iyota, 2022; Moussaoui, Blanco, Muñoz, Raventós,
& Hernández, 2021; Muñoz et al., 2019; Osorio, Moreno, Raventós,
Hernández, & Ruiz, 2018).
First, PSFC has been applied to ethanol–water solutions (Osorio
et al., 2018). In addition, FC has been applied to alcoholic beverages
such as wine, increasing the concentration of alcohol and other mole­
cules such as polyphenols (Petzold, Orellana, Moreno, Cerda, & Parra,
2016) and improving the sensory profile (Wu et al., 2017). More
recently, Osorio et al. (2023) applied falling-film FC to a commercial
Lager beer to modify its sensory profile. Other products obtained by FC
have been applied to the analysis of volatile organic molecules (VOMs),
such as apple juice (Orellana-Palma, Lazo-Mercado, et al., 2020) and
coffee extracts (Moreno et al., 2015).
To the best of our knowledge, no studies have been performed
regarding the impact of FC on beer volatile compounds. Therefore, there
is a research opportunity to study the behaviour of different volatile
organic compounds present in beer and their effect on the sensory
profile in the PSFC process. This paper aims to study the changes in the
sensory profile of three craft ale beers after applying PSFC. Physico­
chemical parameters such as total solids content, ethanol concentration,
total polyphenols, bitterness, colour, and the VOM profile, by its relative
area percent, were evaluated before and after the FC process to deter­
mine the viability of PSFC as a novel process to develop concentrated
beer products from three types of craft ale beer.
2. Methodology
2.1. Sample preparation
Since the “flavour revolution” presents an opportunity for craft ale
beers (Callejo et al., 2020) and colour guides consumers’ categorization
of beer types (Casales-garcia, Gonzalez-abril, Veflen, & Velasco, 2023),
three craft ale beers within the range from pale to dark from Bogotá Beer
Company brewery (BBC, Colombia) were selected: Witbier (pale), Bitter
(amber), and Porter (dark). Before each FC test, the beers were degassed
in a stirred tank at room temperature at 300 rpm for 1 h, as suggested by
texto
Fig. 1. The approximate composition of an average beer by volume percentage (Buiatti, 2008; Verhagen, 2010). The other composition is related to organic volatile
and non-volatile compounds.
2
LWT 191 (2024) 115662
the American Society of Brewing Chemists (ASBC) (ASBC Methods of
Analysis, 2010).
2.2. Progressive stirred freeze concentration protocol
All progressive stirred freeze concentration (PSFC) tests were carried
out with a stirring speed of 300 rpm (Osorio et al., 2018). The freezing
temperature (Tc) for Witbier and Porter was − 15 ◦ C, while that for Bitter
was − 20 ◦ C. PSFC tests were carried out with the same arrangement
used in prior works (Osorio et al., 2018), as shown in Fig. 2. For each
test, 900 g of the degassed sample was used. The Tc was defined ac­
cording to the type of beer. The FC process was performed until an ice
fraction of 0.6 was achieved, from 45 to 75 min. After that, the
concentrated liquid was removed and weighed. Subsequently, the
equipment temperature was increased to 0 ◦ C to separate the ice layer
and defrost at room temperature. The concentrated liquid and ice frac­
tions were separated at the end, and everything described in numerals
2.4 to 2.8 was analysed.
2.3. Data analysis
The summary of the response variables applied to the PSFC is shown
in Table 1.
All the response variables reported in Table 1 were calculated at the
end of the operation at the desired ice fraction. The average ice growth
rate (Eq. 4) was calculated considering mainly the ice conditions (mass,
concentration, and density), heat transfer area and operation time
(Chen, Chen, & Free, 1998; Moreno, Raventós, Hernández, & Ruiz,
2014; Osorio et al., 2018).
2.4. Physicochemical characterization
The physicochemical parameters were measured in triplicate with a
CDR BeerLab® (CDR, Firenze, Italy). This equipment has been used for
several beer studies (Albanese, Ciriminna, Meneguzzo, & Pagliaro,
2017, 2018; Ciriminna et al., 2018; Gernat, Brouwer, Faber-Zirkzee, &
Ottens, 2020; Gernat, Penning, Swinkels, Brouwer, & Ottens, 2020;
Scarano, Pascale, Palladino, Fratini, & Minunni, 2018). Five kits were
used: fermentable sugars (resolution 0.01 g/L), alcohol content (reso­
lution 0.1%), total polyphenols (resolution 1 mg/L), bitterness on the
International Bitterness Unit (IBU) scale (resolution 0.1), and colour on
the Standard Reference Method (SRM) scale (resolution 0.1). In addi­
tion, the total solids content was determined by taking an aliquot of 5 g
and drying it at 60 ◦ C until it reached a constant weight (ISO, 2018;
Osorio et al., 2023).
2.5. Volatile compound analysis
Volatile compound analysis was performed considering the ASBC Beer-
48 (ASBC Methods of Analysis, 2012), with changes suggested by Alves
M. Osorio et al. LWT 191 (2024) 115662

Fig. 2. Experimental setup for progressive stirred freeze concentration (PSFC).

2.6. Sensory analysis

Table 1
Response variables used for progressive stirred freeze concentration.
Sensory profiles were developed by multidimensional approximation
Variable Equation Reference for the original sample, concentrated liquid, and ice fractions of PSFC in
Ice fraction (f) Ice mass (Miyawaki et al., triplicate. Before the sensory analysis, all samples were carbonated using
f= (1)
Initial mass 2012; Nakagawa, DrinkMate® (iDrink, Ann Harbour, USA), bringing the CO2 concentra­
Maebashi, et al.,
tion to saturation and storing the samples at 4 ◦ C.
2010)
Concentration Liquid Solute concentration (Moreno et al., 2014b;
The analysis was developed in two sessions at the certified Labora­
CI = tory for Food Sensory Analysis, Universidad de Antioquia (Medellín,
index (CI) Initial solute concentration
Nakagawa et al.,
Colombia). The analysis was conducted according to ISO 11035, 3972,
2009)
5496, and 8586. The panellists were selected and trained according to
Average Ice Solute concentration (Miyawaki et al.,
Kapp = ISO 8586 (ISO, 2023) and were a group of 4–8 trained judges, both men
distribution Liquid solute concentration 2016; Moreno et al.,
coefficient (Kapp ) (3) 2014a) and women, aged between 25 and 60, in healthy conditions. The set of
Average ice growth
νice =
(Chen et al., 1998; relevant descriptors that gave the maximum information on sensory
rate (νice ) Moreno et al., 2014a; attributes was identified and selected according to the ISO 11035:1994
massice (1 − Solute concentrationice ) Osorio et al., 2018)
standard (ISO, 2015). The reference standard solution for each sensory
time Area densityice
attribute was selected according to ISO 3972 and 5496 (ISO, 2006,
2011). The descriptors were valued on a rating scale of 0–5, except for
and Tian (2020; 2010). All samples (original, liquid, and ice) were global impact, where a scale of 1–3 is used where 3 is high and 1 is low.
extracted by headspace-solid phase microextraction (HS-SPME). For this Likewise, statistically significant differences were determined (p <
purpose, 10 mL of each sample was placed in a 20 mL glass vial, and to 0.05).
improve the extraction efficiency by salting-out, 0.2 g of NaCl was added
and equilibrated for 60 min in the sealed vial at 18 ◦ C with magnetic 2.7. Statistical analysis
stirring. The headspace was collected on a DVB/CAR/PDMS fibre (50/30
μm thickness; Supelco Inc., Bellefonte, PA, USA) over 30 min and directly The freeze concentration tests were performed in triplicate. One-way
injected (5 min desorption time) into an Agilent 7890B gas chromatograph analysis of variance (ANOVA) was applied to the results with a signifi­
coupled to a selective mass detector Agilent 5977A in splitless mode. Mass cance level of 95% with a Tukey test to determine significant differences
spectra were recorded with electronic ionization at 70 eV in the mass between the physicochemical characteristics of each sample and the FC
range 40–300 m/z. An HP-FFAP fused silica column (J&W Scientific, 50 m results. The volatile compound analysis was carried out in triplicate for
× 0.25 mm i.d., 0.32 μm film thickness) was used. The column oven each sample, and ANOVA was applied to the relative area percent for
temperature was programmed to increase from 40 (after 1 min) to 180 ◦ C each compound with a significance level of 95%. A Dunnet test was used
at 1.7 ◦ C/min and then to 220 ◦ C at 30 ◦ C/min. The inlet temperature was to establish the significance of the difference between the concentrated
maintained at 250 ◦ C, and the carrier gas was 1.5 mL of He/min. The linear liquid and the ice fraction regarding the original sample. For the sensory
retention indices were calculated according to the Kovats method using a analysis, ANOVA was applied to the results with a significance level of
mixture of normal paraffin C10–C24 as an external reference. Compound 95%, with a Tukey test to establish the significance of the difference
identification was achieved by matching the query mass spectrum to the between the intensity of the descriptors. The statistical analysis was
reference NIST/EPA/NIH Mass Spectral Library 2014 (2.2) database performed using the Minitab 18 software package (Minitab Inc, Penn­
(acceptance criteria higher than 90%) and by comparing the retention sylvania, USA).
index with those reported in the literature (AM, 2023; NIST Mass Spec­
trometry Data Center, 2006; The Good Scents Company, 2018). All mea­
surements were made in triplicate. The results are shown as the relative
area percent for each compound.

3
M. Osorio et al. LWT 191 (2024) 115662

3. Results
3.1. PSFC results and physicochemical characterization
PSFC was performed on Witbier, Bitter, and Porter up to a 0.6 ice
fraction. The physicochemical characterization of the concentrated
liquid, ice fraction, and original sample are shown in Table 2. The results
of the FC response variables are shown in Fig. 3.
Applying the FC process to the three beers under the conditions
studied was possible. First, the total solid concentration is shown in
Table 2, where Witbier had the highest CI for total solids, with a value of
1.4 (Fig. 2). This beer had the lowest initial concentration. The lowest CI
was for Porter, with a significantly higher initial total solid concentra­
tion than Witbier and Bitter. Accordingly, the highest Kapp was also for
Porter. This could be because an increase in the initial concentration
leads to higher molecular interactions and, thus, lower separation effi­
ciency (Petzold & Aguilera, 2009). Some of the molecules found in the
total solids, such as carbohydrates and peptides, may impact the beer’s
flavour, mainly its sweetness, fullness, mouthfeel, and foam stability
(Depraetere, Delvaux, Coghe, & Delvaux, 2004; Verhagen, 2010). Other
molecules that could be part of these solids are fermentable sugars,
which are highly relevant to the sweetness of beer (Bertuzzi et al., 2020).
The values of fermentable sugars found for Bitter and Porter are
consistent with those reported in other craft beer studies, although those
found for Witbier are slightly lower (Bertuzzi et al., 2020; Preedy, 2008).
Porter also shows the lowest CI for fermentable sugars and the highest
Kapp , possibly because of the interaction of higher molecular weight
compounds from the Maillard reaction (Mosher, 2017; Uald-Lamkad­
dam et al., 2021).
Regarding ethanol, CI values between 1.27 and 1.32 were obtained,
with the highest value for the lowest initial concentration being Witbier,
although there were no significant differences between the beers.
Additionally, ethanol showed higher values of Kapp than total solids and
fermentable sugars, which may occur due to the reinforcement of the
hydrogen bonds by the presence of ethanol (Li et al., 2018), where water
acts as a proton donor and ethanol as a proton receptor (Jiang, Wan,
Zheng, & Xie, 2022). These values are lower than those reported in PSFC
systems in ethanol–water solutions (Osorio et al., 2018) under similar
conditions. The presence of other beer components increases the initial
concentration and molecular interactions: a small number of organic
compounds strengthen the hydrogen bond structure of water-ethanol
(Qin et al., 2022).
Significant differences were found between the CI and Kapp of ethanol
and total solids for Witbier and Bitter, which is evidence of selective
migration, a phenomenon previously described in other matrices’ FC
processes (Dantas et al., 2021; Meneses, Ruiz, Hernandez, & Moreno,
2021; Nakagawa, Maebashi, & Maeda, 2009). These phenomena could
appear due to the difference in the size of the molecules, their diffusivity,
and the occlusion of the system (Vuist, Schutyser, & Boom, 2022; Xu,
Kolliopoulos, & Papangelakis, 2022). Different kinds of chemical com­
pounds are present in beer; however, the main carbohydrates are
maltose and sucrose (Buiatti, 2008). The diffusivity of maltose in water
(between 1.7 and 5% w/w) has been reported to be between 4.8 and 5.1
× 10− 5 cm2/s (Ueadaira & Ueddaira, 1969), while that of sucrose is 4.9
× 10− 5 cm2/s (Hills, Abraham, Hersey, & Bevan, 2011). Ethanol be­
tween 3% and 6% w/w presents higher values, between 5.5 and 6.3 ×
10− 5 cm2/s, in carbonated water-ethanol solutions (Khaireh, Angot,
Cilindre, Liger-Belair, & Bonhommeau, 2021). Although the diffusivity
of ethanol is more remarkable, it presents a higher Kapp value, probably
because the diffusion coefficient of ethanol falls to a minimum as its
concentration increases (Zhang, Wang, Liu, & Zhang, 2006). The size
relationship between ethanol and maltose and the diffusivity values
found show that ethanol should have a lower Kapp value concerning total
solids, which did not occur. This phenomenon can be attributed to solute
premelting, wherein solutes form a solute-rich premelted film around
the ice layer (Uhlmann, Chalmers, & Jackson, 1964). This film is ther­
modynamically stable at temperatures below the bulk melting point and
exhibits remarkable sensitivity to the presence of solutes (Tyagi, Huynh,
Monteux, & Deville, 2020). The concave curvature of the solidification
front plays a crucial role in this process, as it promotes lateral solute
diffusion, causing the front to accelerate and encase the object with the
solute-rich premelted film (Lin, Quan, Cheng, Li, & Chen, 2020).
Consequently, solutes find themselves entrapped within the advancing
ice front despite their higher diffusion rate, owing to the formation of the
premelted film (Saint-Michel, Georgelin, Deville, & Pocheau, 2017;
Tyagi et al., 2020), and therefore leading to a higher occlusion.
However, the values of CI obtained in PSFC were higher than those
reported in beer in falling film FC, although the beers evaluated in this
work have a more complex composition than lagers (Osorio et al., 2023).
It is possible that the agitation system allows for better mass transfer
than the falling film system. The volumetric concentration ratio in the
falling film system is generally not as high. The flowing speed is insuf­
ficient to achieve a high ice purity with sufficient stirring at the ice­
–liquid interface (Miyawaki & Inakuma, 2021).
In addition, the νice for Witbier and Porter was 4.8 and 4.5 μm/s,
respectively, similar to those reported in ethanol–water solutions in the
same FC process (Osorio et al., 2018), while that of Bitter was 6.4 μm/s,
probably because of the difference in the freezing temperature that
causes a higher heat transfer. Some authors have reported a νice value of
8 μm/s as the critical freezing rate (Nakagawa, Nagahama, Maebashi, &
Maeda, 2010; Petzold et al., 2016), so it is possible to confirm that the FC
of the beers was possible under the conditions studied. Ethanol-based
products may require relatively higher freezing rates due to the
depression of the freezing point and the need for a higher heat transfer
rate (Vuist, Boom, & Schutyser, 2020).
For the colour of the beers, the colour changes concerning the orig­
inal sample were greater in the pale beer (Witbier), which makes sense
as it also presented the highest CI value for total solids, where mela­
noidins could be found. This compound comes from nonenzymatic re­
actions and is initially yellow, orange, and red before it turns brown as
the Maillard reaction is allowed to proceed (Bamforth, 2009; Pieczonka
et al., 2021; Van Doorn, Timora, Watson, Moore, & Spence, 2019).

Table 2
Physicochemical characterization of the original sample, concentrated liquid, and ice fraction for Witbier, Bitter, and Porter. Uppercase letters within the same column
denote significant differences (P < 0.05) for each physicochemical parameter.
Beer Fraction Ethanol Total solids %(w/w) Fermentable sugars Colour (SRM) Total Polyphenols (mg/l) Bitterness (◦ IBU)
%(w/w) %(w/w)

Witbier Original 4.12% ± 0.14B 3.65% ± 0.24C 0.42% ± 0.03B 2.5 ± 0.4A 169.3 ± 4B 8.3 ± 0.5A
Liquid 5.45% ± 0.21CD 5.12% ± 0.31DE 0.59% ± 0.05CD 3.5 ± 0.7A 213.5 ± 4C 14.3 ± 0.4B
Ice 2.20% ± 0.57A 1.45% ± 0.07A 0.18% ± 0.06A 1.5 ± 0.8A 100.0 ± 3A 5.6 ± 0.8A
Bitter Original 4.61% ± 0.26BC 3.89% ± 0.07C 0.68% ± 0.02D 11.9 ± 0.8C 305.3 ± 8D 18.8 ± 0.5C
Liquid 5.85% ± 0.36D 5.30% ± 0.28DE 0.98% ± 0.01E 13.5 ± 0.7C 370.0 ± 20E 30.8 ± 1.1E
Ice 2.75% ± 0.21A 1.80% ± 0.28A 0.24% ± 0.06A 8.8 ± 0.4B 208.5 ± 5C 23.4 ± 3.4D
Porter Original 4.14% ± 0.44B 4.73% ± 0.31D 0.63% ± 0.04CD 30.5 ± 1.3E 408.0 ± 7F 18.0 ± 0.8C
Liquid 5.33% ± 0.19CD 6.00% ± 0.42E 0.69% ± 0.01D 36.5 ± 0.7F 438.5 ± 2G 21.0 ± 1.4CD
Ice 2.34% ± 0.2A 2.83% ± 0.24B 0.53% ± 0.01C 26.3 ± 0.4D 375.0 ± 7E 17.4 ± 0.8BC

4
M. Osorio et al.
Fig. 3. Concentration Index (CI) and Average distribution coefficient (Kapp) for Witbier (Yellow-dotted bar), Bitter (Orange-diagonal bar), and Porter (Black-
stripped bar). Uppercase letters denote significant differences (P < 0.05) for each physicochemical parameter. (For interpretation of the references to colour in this
figure legend, the reader is referred to the Web version of this article.)
Although Porter showed the lowest CI for total solids, the colour change
was the second highest, which could be related to the concentration of
polyphenols. In addition to melanoidins, polyphenols can modify the
colour of beer (Bamforth, 2009).
Overall, the total polyphenol concentration was similar to that re­
ported in the literature for similar types of beer (Bertuzzi et al., 2020; D.
O. Carvalho & Guido, 2022; Verhagen, 2010), with Witbier having the
lowest initial concentration of total polyphenols, followed by Bitter and
Porter. Wheat beers usually presented low total polyphenols (Bertuzzi
et al., 2020; Cheiran et al., 2019), allowing a higher concentration at the
liquid fraction (by 1.26 times), the highest increase among the 3 sam­
ples. Bitter has higher initial total polyphenols than Witbier, as expected
due to the higher amount of hops used in this style of beer (Bertuzzi
et al., 2020; Breda, Barros, & Gouvinhas, 2022; D. O. Carvalho & Guido,
2022). Additionally, Porter had the highest initial concentration of
polyphenols, which was expected since some polyphenols have a higher
concentration in dark beers and stout types (Verhagen, 2010). However,
the CI of the total polyphenols of Porter was the lowest due to in­
teractions between melanoidins and the polyphenols.
In this study, only the Witbier had a significant difference in the
original IBU compared to the Bitter and the Porter. It allows a higher
increase in bitterness related to the other styles. Porter had the lowest
IBU increase (1.17 times), possibly due to the occlusion of these mole­
cules caused by the chemical interaction with proteins (Bamforth, 2009)
that could also be trapped in the ice, with Porter being the style with the
highest concentration of total solids. The litter liquid fraction has the
highest IBU value statically, probably because of the lower occlusion of
proteins compared to Porter.
In general, the freezing temperatures used in this study allowed
similar ethanol CIs to be obtained for the three types of beer, while the
solids were only different for Porter beer (which had the highest initial
solid content). The CI and Kapp reached for the other physicochemical
parameters were significantly different since these are more distinctive
in each type of beer. Furthermore, the occlusion of Porter beer solids led
to a higher occlusion in fermentable sugars and total polyphenols,
possibly due to the interactions between these molecules.
3.2. Volatile analysis
The volatile organic molecules (VOMs) of the initial extract, the
liquid, and the ice fractions of PSFC of three beer styles were identified
and quantified through GC–MS. Fig. 4 shows the representative chro­
matogram of the original sample of Witbier, Bitter and Porter. Table 3
5
LWT 191 (2024) 115662
shows the experimental retention index (RI), literature value of RI, odor
note, and the relative amount in each sample (% area percentage).
ANOVA was applied with Dunnet’s test to find significant differences in
the relative composition by the area percentage of each compound in the
concentrated liquid and the ice fraction to the original sample (p <
0.05). The type of VOMs were alcohols (30%), followed by esters (26%),
terpenes (17%), and furan and ketones (9% each); the remaining
composition corresponded to an aldehyde and a carboxylic acid. This
distribution is similar to that reported by Alves et al. (2020), showing a
higher predominance of higher alcohols, those containing more carbon
atoms than ethanol (Colicchio et al., 2011), and a lower presence of
aldehydes.
In addition to ethanol, beer contains several alcohols derived mainly
from yeast metabolism and hops and malts, commonly known as higher
alcohols. These compounds are formed as byproducts of amino acid
synthesis and catabolism (Olaniran, Hiralal, Mokoena, & Pillay, 2017),
usually exhibit intense aromas, and can warmly affect taste. Higher al­
cohols are the direct precursors of esters and contribute to favourable
beer flavour (Verhagen, 2010). They also may contribute to beer texture
in the mouth (mouthfeel), and floral aromas from some of these
contribute to the pleasing aroma (Buiatti, 2008). Some of the most
relevant alcohols were 3-methyl-1-butanol and phenylethyl alcohol. All
alcohols and acids present in beer are theoretically capable of esterifi­
cation reactions, creating many esters (Buiatti, 2008). Overall, esters
give the beer a fruity character (Verhagen, 2010). Some of the most
common esters in beer are 3-methyl-butyl acetate, ethyl hexanoate,
ethyl octanoate, and phenylethyl acetate (Alves et al., 2020; Buiatti,
2008; Verhagen, 2010). Conversely, terpenes are natural compounds
primarily from the hop and in minor proportion from malt (Buiatti,
2008). Additionally, terpene and lipid degradation pathways may
interact to form new terpenes (Bettenhausen et al., 2018). Furthermore,
in most beer, terpenes are associated with floral and fruity notes, and
some of the most common are β-myrcene and linalool (Bettenhausen
et al., 2018; Eyres & Dufour, 2008; Martins, Brandão, Almeida, & Rocha,
2018). Other VMOs in beer are carbonyl compounds, such as aldehydes
and ketones, and are essential for the quality of the beer because some of
them are characterized as possible off-flavours (Bamforth, 2009), while
compounds such as Furans constitute a significant class of compounds
formed during the Maillard reactions (Alves et al., 2020).
Fig. 5 shows the VOMs in Witbier fractions. In the original sample,
approximately 52% of the area corresponds to esters, the most pre­
dominant compounds for Witbier, possibly due to the presence of wheat
in its fabrication, which gives the beer more unique aromatic
M. Osorio et al.
Fig. 4. GC analyses on DB-FFAP column of volatile compounds from Witbier (A), Bitter (B), and Porter (C) original beers (without concentration) obtained by HS-
SPME. Peak numbers correspond to the compound numbers in Table 3.
compounds (Villacreces et al., 2022). Among these compounds, ethyl
octanoate has the highest relative composition, the same as that re­
ported in Lager beer by Alves et al. (2020). Ethyl octanoate has been
highly associated with fruity and floral notes in beer, while ethyl hex­
anoate and heptanoate have also been associated with wine–brandy
notes. In addition, terpenes occupy 20% of the area, mainly by linalool,
6
LWT 191 (2024) 115662
which is a suitable marker compound for hoppy floral flavour, and in
minor proportion by citronellol (floral, citrus aroma) and limonene,
with citrus notes, which are very characteristic of Witbier beers (Strong,
2021). Witbier had the highest terpene relative concentration among the
three beers. Higher alcohols represent approximately 15% of the total
area, with the major participation of 3-methyl-1-butanol (whiskey,
M. Osorio et al. LWT 191 (2024) 115662

Table 3
VOMs distribution by relative area percentage in GC analysis for each type of beer and fraction evaluated.
A
Peak Compound CAS RI Cal RI Lit Flavor Relative percentage area
B
Number Category
Witbier Bitter Porter

Original Liquid Ice Original Liquid Ice Original Liquid Ice

1 2-Methyl-3- 565-69- 1025 1003 Herbal, mint 0.67 ± 0.64 1.00 1.47 ± 1.14 1.40 1.35 ± 0.84 1.14
pentanone 5 0.14 ± 0.10 ± 0.16 ± ± 0.09 0.06 ± 0.07 ± 0.65
0.14* 0.09*
2 3-Methyl-butyl 123-92- 1111 1128 Fruity, apple, 6.30 ± 6.62 11.30 10.68 ± 9.86 10.15 15.50 ± 11.23 12.36
acetate 2 banana-like 2.95 ± 1.40 ± 3.64 2.61 ± 1.31 ± 3.21 2.91 ± 0.94 ±
11.22
3 β-Myrcene 123-35- 1143 1158 Herbal, 0,02 ± 0.06 0.06 0.14 ± 0.11 0.10 0.44 ± 0.23 0.48
3 metallic, 0,03 ± 0.02 ± 0.06 0.07 ± 0.09 ± 0.04 0.06 ± 0.05 ± 0.57
spicy, fruity,
woody
4 Limonene 138-86- 1180 1206 Citrus, green, 0.35 ± 0.25 0.22 0.21 ± 0.20 0.22 0.31 ± 0.14 0.29
3 lemon-like 0.25 ± 0.06 ± 0.19 0.03 ± 0.06 ± 0.06 0.04 ± ± 0.06
odor. 0.08*
5 3-Methyl-1- 123-51- 1206 1209 Alcohol, 8.60 ± 8.75 14.58 19.44 ± 17.88 20.02 18.24 ± 14.57 24.30
butanol 3 malty, burnt, 1.80 ± 0.94 ± 3.69 ± 1.60 ± 1.87 0.13 ± 1.67 ± 9.09
banana-like 0.16*
6 Ethyl hexanoate 123-66- 1223 1226 Fruity, 8.97 ± 9.67 13.51 19.32 ± 17.65 19.82 22.54 ± 15.27 9.09
0 strawberry- 2.74 ± 1.55 ± 3.43 ± 2.21 ± 3.66 0.70 ± 5.61 ±
like 1.14* 7.22*
7 1-Pentanol 71-41-0 1248 1253 Balsamic, 0±0 0.03 0.35 2.67 ± 1.51 1.30 1.04 ± 0.41 1.07
fusel-like ± 0.05 ± 0.60 3.14 ± 1.03 ± 1.02 1.60 ± 0.44 ± 1.41
sweet
8 Hexyl acetate 142-92- 1262 1268 Fruity, green 0.19 ± 0.16 0.22 0.19 ± 0.19 0.17 0.41 ± 0.37 0.07
7 0.02 ± 0.05 ± 0.02 0.06 ± 0.03 ± 0.03 0.11 ± 0.26 ± 0.06
9 Ethyl heptanoate 106-30- 1321 1327 Fruity, berry 0.11 ± 0.11 0.11 1.29 ± 1.45 1.61 1.21 ± 1.26 0.08
9 0.01 ± 0.01 ± 0.05 1.01 ± 0.58 ± 0.68 0.52 ± 0.46 ±
0.07*
10 6-Methyl-5- 110-93- 1328 1319 Mushroom, 0,02 ± 0±0 0±0 0.26 ± 0.18 0.08 0.11 ± 0.08 0.02
hepten-2-one 0 earthy 0,03 0.23 ± 0.19 ± 0.02 0.04 ± 0.03 ±
0.03*
11 1-Hexanol 111-27- 1345 1355 Fruity fatty, 0.08 ± 0.08 0.05 0.21 ± 0.13 0.29 0.17 ± 0.09 1.13
3 herbal 0.02 ± 0.01 ± 0.09 0.10 ± 0.02 ± 0.07 0.03 ± 0.08 ± 1.85
12 1,2-Dimethyl- Not 1351 1367 Not reported 0.01 ± 0±0 0.03 0.15 ± 0.19 0.16 4.16 ± 4.86 1.11
cyclopent-2-ene- reported 0.01 ± 0.05 0.05 ± 0.07 ± 0.04 0.57 ± 0.54 ±
carboxylic acid 0.75*
13 Ethyl octanoate 106-32- 1437 1435 Fruity, 36.06 ± 31.17 11.91 1.68 ± 16.59 12.86 6.54 ± 16.23 8.24
1 pineapple- 6.57 ± 4.58 ± 0.51 ± ± 5.35 ± 4.70 ±
like 4.27* 8.15* 2.01* 12.86
14 1-Heptanol 111-70- 1456 1454 Leafy, green 0.23 ± 0.52 0.18 0.73 ± 0.63 1.12 0.45 ± 0.19 0.28
6 0.33 ± 0.64 ± 0.12 0.48 ± 1.05 ± 0.75 0.50 ± 0.15 ± 0.37
15 2-Ethyl hexenal 645-62- 1484 1491 Bitter, rancid 0.24 ± 0.23 0.65 0.40 ± 0.35 0.46 0.11 ± 0.30 0.30
5 0.06 ± 0.07 ± 0.58 0.16 ± 0.05 ± 0.08 0.14 ± 0.07 ± 0.18
16 2-Acetyl-furan 1192- 1496 1497 Sweet, 1.38 ± 1.34 1.04 0.07 ± 0.07 0.05 0.42 ± 0.53 0.63
62-7 balsamic, 0.29 ± 0.29 ± 0.69 0.07 ± 0.06 ± 0.04 0.21 ± 0.27 ± 0.19
burnt, nutty
17 Linalool 78-70-6 1543 1540 Fruity, floral, 19.44 ± 14.73 29.27 3.23 ± 3.77 3.55 1.84 ± 1.51 1.88
muscat lemon 3.95 ± 2.89 ± 0.27 ± 0.47 ± 0.85 0.59 ± 0.22 ± 0.50
2.01*
18 1-Octanol 111-87- 1552 1554 Fatty, sweet, 0.76 ± 1.04 0.06 0.32 ± 0.81 0.99 0.95 ± 0.41 0.39
5 fruity 0.78 ± 0.87 ± 0.11 0.20 ± 0.31 ± 0.46 ± 0.21 ± 0.07
0.02*
19 2-Furanmethanol 98-00-0 1643 1650 Caramel, 2.12 ± 2.23 0.02 0.19 ± 0.11 0.18 0.86 ± 0.88 1.16
burnt sugar, 3.10 ± 1.40 ± 0.03 0.04 ± 0.03 ± 0.07 0.15 ± 0.06 ± 0.24
creamy
20 1-Nonanol 143-08- 1672 1666 Fatty, citrus, 0.45 ± 0.94 0.18 3.39 ± 1.19 0.91 0.47 ± 1.02 1.19
8 orange 0.08 ± 1.04 ± 0.19 3.40 ± 1.69 ± 0.76 0.52 ± 1.52 ± 1.69
21 Citronellol 106-22- 1769 1762 Floral, rose, 0.36 ± 0.54 0.42 0.53 ± 0.44 0.43 0.40 ± 0.47 0.35
9 citrus 0.05 ± 0.24 ± 0.06 0.08 ± 0.08 ± 0.07 0.06 ± 0.04 ± 0.17
22 2-Phenylethyl 103-45- 1808 1810 Floral, rose, 0.77 ± 0.89 0.84 1.12 ± 1.12 0.97 1.23 ± 1.31 0.89
acetate 7 fruity 0.12 ±0 ± 0.10 0.16 ± 0.10 ± 0.06 0.04 ± 0.16 ±
0.20*
23 2-Phenylethanol 60-12-8 1899 1903 Floral, sweet, 5.29 ± 6.11 6.45 14.01 ± 13.70 12.79 10.01 ± 12.87 13.43
honey 0.99 ± 0.49 ± 0.80 3.28 ± 2.05 ± 1.54 1.27 ± 0.86 ± 2.31
A
RI (Retention Index) (AM, 2023; NIST Mass Spectrometry Data Center, 2006; The Good Scents Company, 2018) B Flavor category The Good Scent Company and
Pherobase (AM, 2023; The Good Scents Company, 2018) * Represents significative differences between the original sample and the evaluated fraction (p < 0.05).

malty, burnt) and 2-phenylethanol (floral, alcohol, honey). 1-Nonanol caramel, sugarcane, and burnt sugar, respectively (AM, 2023; ASBC
and 1-octanol are associated with orange peel notes, a key ingredient Methods of; Analysis, 2017; Burdock, 2005).
in Witbier production (Strong, 2021). The furans found in the Witbier After the PSFC process, the relative distribution of VOMs in Witbier
were 2-acetylfuran and 2-furanmethanol, related to coffee, burnt, nutty, was preserved for the concentrated liquid. However, two compounds

7
M. Osorio et al.
Fig. 5. VOMs profile by the chemical group in the original sample, concentrated liquid, and ice fraction of Witbier, Bitter, and Porter by area percentage of the GC-
MS spectra.
were no longer detected: 6-methyl-5-hepten-2-one and 1,2-dimethyl-
cyclopent-2-ene-carboxylic acid. On the other hand, at the ice fraction,
26% of the total VOMs in the original sample had a significant change.
The proportion of esters decreased by approximately 14% compared to
the original sample, mainly because of a significant increase in ethyl
octanoate. In addition, the relative composition of 3-methyl-1-butanol,
ethyl hexanoate, 2-methyl-3-pentanone, and linalool significantly
changed. Finally, 6-methyl-5-hepten-2-one was no longer detected in
the ice fraction.
On the other hand, the original Bitter sample presents a predomi­
nance of higher alcohol VOMs, nearly 40% by relative concentration,
mainly from 3-methyl-1-butanol (19%) and 2-phenylethanol (14%),
which have been reported to independently contribute to the overall
beer aroma (Kishimoto, Noba, Yako, Kobayashi, & Watanabe, 2018). It
also has a higher relative amount of 1-hexanol, 1-heptanol, and 1-non­
anol than Witbier beer, which is related to an alcoholic, fatty, green
flavour. Additionally, it has 1-pentanol, an aliphatic alcohol produced
by yeast with a pleasant odor and burning taste (Burdock, 2005; Tang &
Li, 2017). The esters represent 34.3% of the total area, mainly from ethyl
hexanoate and 3-methyl-butyl acetate. However, Bitter beer had the
8
LWT 191 (2024) 115662
lowest relative concentration of esters compared to Witbier and Porter.
Terpenes also had a significantly lower proportion than Witbier,
although β-myrcene was detected in the original sample. This compound
has been associated with the ripeness of the hops and is a potent
odourant in beer (Briggs, Boulton, Brookes, & Stevens, 2004), with a
resinous, spicy aroma, which is distinctive for a Bitter style (ASBC
Methods of Analysis, 2017; Piggott, 2012; Strong, 2021). At the
concentrated liquid fraction, there was a significant change in the
relative concentration of two compounds: ethyl octanoate increased its
participation, while 2-methyl-3-pentanone decreased it to the original
sample. On the other hand, ethyl octanoate and 1-octanol increase their
relative concentrations at the ice fraction. Overall, 91% of the VOMs’
relative abundance was preserved in both fractions.
Finally, Porter showed a higher proportion of esters (47.3%), fol­
lowed by higher alcohols (31.3%). The major relative concentration in
esters was related to ethyl hexanoate and 3-methyl-butyl acetate (22.5
and 15.5%, respectively), while in alcohols were 3-methyl-1-butanol
and 2-phenylethanol, with 18.2% and 10%, respectively. These four
compounds were also reported as the most abundant VOMs in a Belgian
Dark Strong Ale, another dark beer from the Ale family (Coelho et al.,
M. Osorio et al.
2019). It also presented a higher relative concentration of 1,2-dimethyl-­
cyclopent-2-ene-carboxylic acid, an acid compound with no reported
flavour, that had been found in sorghum beer and wine made from goji
berries (Budner et al., 2021; Yuan et al., 2016). The lower proportion of
terpenes related to Witbier could be explained by using dark malts in the
production of Porter because terpenes are significantly higher in pale
beers than in dark beers (Paszkot, Gasiński, & Kawa-Rygielska, 2023).
Ninety-six percent of the VOMs preserve their relative abundance in the
concentrated liquid, with only a significant decrease in the limonene
relative concentration. In addition, at the ice fraction, five compounds
had a significant decrease in their relative concentration: ethyl hepta­
noate, ethyl hexanoate, 1,2-dimethyl-cyclopent-2-ene-carboxylic acid,
2-phenylethyl acetate, and 6-methyl-5-hepten-2-one, leading to a sig­
nificant change of 22% in the VOM relative concentration.
Several authors have shown the ability of various FC techniques to
maintain the volatile profile in coffee and fruit beverages (Moreno et al.,
2015; Orellana-Palma, Lazo-Mercado, et al., 2020; Orellana-Palma,
Tobar-Bolaños, et al., 2020; Ramos, Delgado, Bautista, Morales, &
Duque, 2005). This work shows the PSFC potential to preserve (the
concentrated liquid of three beers) and modify (the ice fraction of
Witbier and Porter) the relative concentration of VOMs of three Ale
beers. It was achieved by not rehydrating the original sample, evaluating
the concentrated product, and the fraction of ice recovered. A similar
result was found by Wu et al. (2017) in Cabernet Sauvignon Wine, where
FC led to higher amounts of esters and higher alcohols as well as a lower
volatile acid content. The effect of changes in WOMs on the sensory
profiles of the samples had to be evaluated. These results are shown in
Section 3.3.
3.3. Sensory analysis
The sensory analysis of the original sample of the three types of beer
was carried out, and it was compared with the profiles of the concen­
trated liquids and the ice fractions obtained from each one after the
PSFC process. In addition, the sensory profiles were associated with the
volatile compounds detected in Section 3.2 and the information in
Table 2.
First, in Fig. 6, the sensory profile of the original sample of Witbier
beer can be observed. This beer shows a balanced aromatic profile, with
similar values for alcohol, malty, sweet, floral, and hoppy notes, with
slightly lower fruit and acid notes. Regarding flavour, this sample
Fig. 6. Sensory profile of the original sample of Witbier (Bars) vs. concentrated liquid (Continuous green line) and ice fraction (Blue dotted line). Significant dif­
ferences p < 0.05 for concentrated liquid are Diamonds and Squares for ice fraction, relative to the original sample. The abbreviation corresponds to Odor (O), Taste
(T), and somatosensory (SS). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)
9
LWT 191 (2024) 115662
showed sweet, floral, fruity, hoppy, and alcoholic flavours, with less
intense notes of acid and malt. This profile could be associated with a
higher proportion of esters and terpenes (Bettenhausen et al., 2018;
Paszkot et al., 2023; Sharp, Steensels, & Shellhammer, 2017). Addi­
tionally, it was possible to identify green and tobacco-related flavours
related to hexyl acetate and 2-phenylethyl acetate, respectively. Alcohol
flavours and aromas are not only due to the ethanol in the beer but also
to 3-methyl-1-butanol and 2-phenylethanol. In addition, floral notes can
be associated with 2-phenylethyl acetate and citronellol, while fruity
notes are mainly associated with the esters ethyl hexanoate and ethyl
heptanoate. Ethyl octanoate and linalool give floral and fruity flavours,
which had the major participation in the GC area (Table 3). The
sweetness could be related mainly to the fermentable sugars discussed in
Section 3.1. Additionally, Witbier presented the lowest intensity in this
descriptor among the three beers, being the one with the lowest ◦ IBU. In
this same sense, although polyphenols have no aroma, they impact
several beer characteristics, such as astringency, haze, colour, and body
(Colicchio et al., 2011). Witbier presented the least astringency, with the
lowest total polyphenol content associated with this characteristic (Aron
& Shellhammer, 2010).
Nine of the twenty-three descriptors significantly increased in the
concentrated liquid compared to the original sample. Although the
relative composition of the VOMs did not significantly change, it is
possible that an increase in the concentration of the molecules occurred
but maintained the same distribution, thus increasing the flavour in­
tensity. In addition, the rise in the hop aroma could be associated with
increased alfa acids related to the IBUs. The increase in total solids raises
the beer’s body, highlighting the malty flavours, just as the increase in
fermentable sugars presented an increase in the sweet flavour. Finally,
the increase in total polyphenols was reflected in a significant increase in
astringency. Although several descriptors significantly changed, the
global impact still presented the highest value (3), possibly by main­
taining the distribution of VOMs. In the ice fraction, the decrease in the
intensity of fruity aroma and floral taste could be associated with the
significant decrease in the participation of ethyl octanoate (de Lima,
Aceña, Mestres, & Boqué, 2023; Yang et al., 2022). The malty and sweet
taste increase could be related to the increase in the relative area of
3-methyl-1-butanol (Coelho et al., 2019). Additionally, the occlusion of
total solids may allow for maintaining the beer’s body. Even though the
ice fraction has a lower concentration of all physicochemical parameters
and a decrease in three sensory descriptors compared to the original
M. Osorio et al.
sample, it maintains its global impact at the highest value. Its new VOM
profile may have made this an attractive light beer.
Fig. 7 shows that Bitter is a more complex beer than Witbier. It has
more malty, alcoholic, and sweet aromas, possibly because of the higher
proportion of higher alcohols, mainly 3-methyl-1-butanol, 2-phenyl­
ethanol, and 1-pentanol, associated with alcoholic, malty, honey, and
sweet notes (ASBC Methods of Analysis, 2017; Coelho et al., 2019;
Kishimoto et al., 2018). It also had a major proportion of ethyl hex­
anoate (rather than the ethyl octanoate in Witbier), which has more
wine and brandy aromas (de Lima et al., 2023; Yang et al., 2022). Its
taste is characterized by a strong bitterness, being the beer with the
highest initial ◦ IBU; its higher ethanol content compared to the Witbier
and predominant green notes in the flavour, possibly associated with the
6-methyl-5-hepten-2-one (de Lima et al., 2023). This description cor­
responds to that expected for this type of beer, given that the balance
may vary fairly, even between malt and hops, and may be somewhat
bitter (Strong, 2021). The concentrated liquid showed a significant in­
crease in three descriptors (yeast flavour, tobacco flavour, and astrin­
gent sensation) and decreased malty aroma. As in Witbier, the increase
in astringency can be explained by the increase in total polyphenols in
the sample. The increase in tobacco flavour could be related to changes
in 2-phenylethyl acetate. An increase in green flavour was obtained in
the ice fraction, possibly related to 1-heptanol. The fruity flavour is
related to the increase in the 1-octanol and ethyl octanoate proportion
(Coelho et al., 2019). The most marked change in the VOM profile be­
tween the original and the liquid and ice fractions was the increase in the
relative abundance of ethyl octanoate, which may be the cause of the
reduction in the global impact of both fractions because it has been re­
ported that when this compound exceeds its threshold, it gives the beer
an undesirable flavour (Olaniran et al., 2017).
Finally, Fig. 8 shows that the higher descriptors of Porter are
bitterness and body, which makes sense since this beer had a higher
value of total solids concentration and an IBU similar to the Bitter beer.
2-Ethyl hexenal may contribute to the bitter flavour (Burdock, 2005).
The green taste could be associated with 1-hexanol, 1-heptanol, hexyl
acetate, 6-methyl-5-hepten-2-one, and limonene, while the roasted taste
is related to furans, 2-acetyl-furan, and 2-furanmethanol (ASBC Methods
of Analysis, 2017; Burdock, 2005). The alcohol taste came from ethanol
and higher alcohols (ASBC Methods of Analysis, 2017; Burdock, 2005).
Nineteen descriptors were maintained in the concentrated liquid, while
the remaining 3 significantly decreased, although Table 3 shows that all
Fig. 7. Sensory profile of an original sample of Bitter (Bars) vs. concentrated liquid (Continuous green line) and ice fraction (Blue dotted line). Significant differences
p < 0.05 for concentrated liquid are Diamonds and Squares for ice fraction, relative to the original sample. The abbreviation corresponds to Odor (O), Taste (T), and
somatosensory (SS). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)
10
LWT 191 (2024) 115662
physicochemical characteristics increased. Dark beer perception could
be affected by its colour because it is expected to be more bitter, have a
higher alcohol content, and have more body than pale beer (F. R. Car­
valho, Moors, Wagemans, & Spence, 2017; Reinoso-Carvalho, Dakduk,
Wagemans, & Spence, 2019). The colour rise in concentrated liquid may
generate a higher expectation of bitterness, alcohol content, and body,
generating a lower score for not meeting these expectations (Reinoso-­
Carvalho et al., 2019). At the ice fraction, 14 of the 22 descriptors were
preserved, while the aroma acid rose and the other 8 descriptors were
significantly reduced: sweet and roasted aroma, bitter, alcohol, green,
roasted taste, and the body.
The global impact of the samples was evaluated from 0 to 3 and is
shown in Figs. 4–6. The Witbier beer obtained a value of 3, its concen­
trated liquid, and the ice fraction. It opened an opportunity to develop
new products for this type of beer: creating two fractions with different
sensory profiles and changes in the physicochemical properties and
volatile composition was achieved, and the global impact was still
preserved. A similar case occurred for the Porter, where the global
impact was preserved for the concentrated liquid and the ice fraction.
The Bitter beer global impact decreased from 3 to 2 in the concentrated
liquid and ice fractions. This is likely due to their characteristics: the
balance can range from fairly even between malt and hops to somewhat
bitter, and its drinkability is critical to the style (Strong, 2021). Previous
works presented the viability of applying FC to modify the sensory
profile of Lager beer (Osorio et al., 2023). However, this is the first study
to apply a VOM profile and to the ice fraction to relate it to sensory
changes and changes in physicochemical characteristics. The changes in
sensory profiles show the possibility of applying FC to develop beer
products.
4. Conclusions
Progressive stirred freeze concentration was successfully applied to
three types of craft beers: Witbier, Bitter, and Porter. The concentrated
liquids obtained after PSFC from the three beers increased the ethanol
content, total solids, total polyphenols, and fermentable sugars and
changed the colour and bitterness compared to the original sample.
Additionally, the freeze-concentrated beer products presented changes
in the relative composition of the volatile components by area per­
centage in GC analysis, with Witbier changing the most, mainly in al­
cohols and esters. Likewise, the products obtained sensory profiles
M. Osorio et al.
Fig. 8. Sensory profile of an original sample of Porter (Bars) vs. concentrated liquid (Continuous green line) and ice fraction (Blue dotted line). Significant differences
p < 0.05 for concentrated liquid are Diamonds and Squares for ice fraction, relative to the original sample. The abbreviation corresponds to Odor (O), Taste (T), and
somatosensory (SS). (For interpretation of the references to colour in this figure legend, the reader is referred to the Web version of this article.)
different from the original ones, linked to the physicochemical and
volatile changes.
However, the physicochemical characteristics found in the recovered
ice fractions are still within the quality parameters defined for each type
of beer due to the occlusion phenomena, where changes in the relative
concentration of VOMs were found and related to changes in the sensory
profile. Hence, both fractions obtained after applying PSFC show the
potential to be commercialized.
This presents an opportunity to develop new beer products by
applying freeze concentration technology since both a concentrated and
a lighter product were possible with different sensory profiles and with
changes in the physicochemical properties and volatile distribution.
Consent to participate in the publication
The authors approve the publication and their respective participa­
tion in this research without restriction.
CRediT authorship contribution statement
M. Osorio: Formal analysis, Investigation, Methodology, Visualiza­
tion, Writing – original draft. F.L. Moreno: Formal analysis, Supervi­
sion, Writing – review & editing. E. Hernández: Formal analysis,
Supervision, Writing – review & editing. Annamaria Filomena-
Ambrosio: Formal analysis, Writing – review & editing. Coralia Osorio:
Formal analysis, Writing – review & editing. Y. Ruiz: Conceptualization,
Funding acquisition, Project administration, Supervision, Writing – re­
view & editing, Formal analysis.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
11
LWT 191 (2024) 115662
Acknowledgements
Funding:
This work was supported by Universidad de La Sabana under the
project ING-263-2020. Manuel Osorio thanks Universidad de La Sabana
for the Carlos Jordana Distinction. We are grateful to engineers Ale­
jandra Orjuela and Mariana Guzman, for their support in the experi­
mentation and logistics.
References
Albanese, L., Ciriminna, R., Meneguzzo, F., & Pagliaro, M. (2017). Beer-brewing powered
by controlled hydrodynamic cavitation: Theory and real-scale experiments. Journal
of Cleaner Production, 142, 1457–1470. https://doi.org/10.1016/J.
JCLEPRO.2016.11.162
Albanese, L., Ciriminna, R., Meneguzzo, F., & Pagliaro, M. (2018). Innovative beer-
brewing of typical, old and healthy wheat varieties to boost their spreading. Journal
of Cleaner Production, 171, 297–311. https://doi.org/10.1016/J.
JCLEPRO.2017.10.027
Almeida, É. da S., Arend, G. D., Knapp, M. A., Rezzadori, K., Verruck, S., Hotza, D., et al.
(2023). Effect of the multi-stage block freeze concentration process on the
physicochemical and biological properties of noni tea (Morinda citrifolia L.): A case
study in Brazil to obtain a promising functional food. Journal of Food Measurement
and Characterization. https://doi.org/10.1007/S11694-022-01719-1
Alves, V., Gonçalves, J., Figueira, J. A., Ornelas, L. P., Branco, R. N., Câmara, J. S., et al.
(2020). Beer volatile fingerprinting at different brewing steps. Food Chemistry. ,
Article 126856. https://doi.org/10.1016/j.foodchem.2020.126856
Am, E.-S. (2023). The Pherobase: Database of Pheromones and semiochemicals. The
Pherobase. https://www.pherobase.com/.
Aquilani, B., Laureti, T., Poponi, S., & Secondi, L. (2015). Beer choice and consumption
determinants when craft beers are tasted: An exploratory study of consumer
preferences. Food Quality and Preference, 41, 214–224. https://doi.org/10.1016/j.
foodqual.2014.12.005
Aron, P. M., & Shellhammer, T. H. (2010). A discussion of polyphenols in beer physical
and flavour stability. Journal of the Institute of Brewing, 116(4), 369–380. https://doi.
org/10.1002/j.2050-0416.2010.tb00788.x
ASBC Methods of Analysis. (2010). Recommended beer degassing methods and
alternatives matrix. Journal of the American Society of Brewing Chemists, 41, 2–5.
https://doi.org/10.1094/ASBCMOA-Beer-1
ASBC Methods of Analysis. (2012). Headspace gas chromatography-flame ionization
detector analysis for beer volatiles - beer 48. Journal of the American Society of
Brewing Chemists, 70(4), 321–323. https://doi.org/10.1094/ASBCJ-2012-1101-05
ASBC Methods of Analysis. (2017). American society of brewing Chemists flavor database.
http://methods.asbcnet.org/Flavors_Database.aspx.
Bamforth, C. W. (2009). Handbook of alcoholic beverages series: Beer a quality perspective
(Vol. 6, p. 347). Elsevier Ltd. http://books.google.com/books?hl=en&lr=&id=2UqC
FxskEnMC&oi=fnd&pg=PP2&dq=Beer+a+quality+perspective&ots=fkcer_CaY_&s
ig=mRdaHljcl2uKtBY4OS2jGto9DAc.
Barros, E. L. da S., Silva, C. C., Canella, M. H. M., Verruck, S., Prestes, A. A.,
Vargas, M. O., et al. (2021). Effect of replacement of milk by block freeze
M. Osorio et al.
concentrated whey in physicochemical and rheological properties of ice cream. Food
Science and Technology, 42. https://doi.org/10.1590/FST.12521
Bertuzzi, T., Mulazzi, A., Rastelli, S., Donadini, G., Rossi, F., & Spigno, G. (2020).
Targeted healthy compounds in small and large-scale brewed beers. Food Chemistry,
310, Article 125935. https://doi.org/10.1016/j.foodchem.2019.125935
Bettenhausen, H. M., Barr, L., Broeckling, C. D., Chaparro, J. M., Holbrook, C., Sedin, D.,
et al. (2018). Influence of malt source on beer chemistry, flavor, and flavor stability.
Food Research International, 113, 487–504. https://doi.org/10.1016/j.
foodres.2018.07.024
Breda, C., Barros, A. I., & Gouvinhas, I. (2022). Characterization of bioactive compounds
and antioxidant capacity of Portuguese craft beers. International Journal of
Gastronomy and Food Science, 27(January), Article 100473. https://doi.org/
10.1016/j.ijgfs.2022.100473
Briggs, D. E., Boulton, C. A., Brookes, P. A., & Stevens, R. (2004). Brewing: Science and
practice. In Brewing: Science and practice. Woodhead Publishing Limited. https://doi.
org/10.1533/9781855739062.
Budner, D., Carr, J., Serafini, B., Tucker, S., Dieckman-meyer, E., Bell, L., et al. (2021).
Statistical significant differences between aroma profiles of beer brewed from
sorghum. Beverages, 7(3), 1–11. https://doi.org/10.3390/beverages7030056
Buiatti, S. (2008). Beer composition: An overview. In Beer in health and disease prevention
(pp. 213–225). Elsevier. https://doi.org/10.1016/b978-0-12-373891-2.00020-1.
Burdock, G. (2005). In Fenaroli’s handbook of flavor ingredients (6◦ Edition). New York.
Callejo, M. J., Tesfaye, W., & Morata, A. (2020). Chapter 5. Craft beers: Current situation
and future trends. In New advances on fermentation processes. https://books.google.
com.co/books?hl=es&lr=&id=1pj8DwAAQBAJ&oi=fnd&pg=PA83&dq=craft+
beer+vs+industrial+beer+composition&ots=nHjSsyJiRo&sig=lcn
xJH5Ir27dOTY-GcpyCXij5Q0&redir_esc=y#v=onepage&q=craft beer vs industrial
beer composition&f=false.
Carvalho, D. O., & Guido, L. F. (2022). A review on the fate of phenolic compounds
during malting and brewing: Technological strategies and beer styles. Food
Chemistry, 372, Article 131093. https://doi.org/10.1016/J.
FOODCHEM.2021.131093
Carvalho, F. R., Moors, P., Wagemans, J., & Spence, C. (2017). The influence of color on
the consumer’s experience of beer. Frontiers in Psychology, 8(DEC). https://doi.org/
10.3389/fpsyg.2017.02205
Casales-garcia, V., Gonzalez-abril, L., Veflen, N., & Velasco, C. (2023). Assessing the
influence of colour and glass type on beer expectations. Food Quality and Preference,
103(May 2022), Article 104701. https://doi.org/10.1016/j.foodqual.2022.104701
Cheiran, K. P., Raimundo, V. P., Manfroi, V., Anzanello, M. J., Kahmann, A.,
Rodrigues, E., et al. (2019). Simultaneous identification of low-molecular weight
phenolic and nitrogen compounds in craft beers by HPLC-ESI-MS/MS. Food
Chemistry, 286(February), 113–122. https://doi.org/10.1016/j.
foodchem.2019.01.198
Chen, P., Chen, X. D., & Free, K. W. (1998). Solute inclusion in ice formed from sucrose
solutions on a sub-cooled surface—an experimental study. Journal of Food
Engineering, 38(1), 1–13. https://doi.org/10.1016/S0260-8774(98)00112-5
Ciriminna, R., Albanese, L., Di Stefano, V., Delisi, R., Avellone, G., Meneguzzo, F., et al.
(2018). Beer produced via hydrodynamic cavitation retains higher amounts of
xanthohumol and other hops prenylflavonoids. LWT, 91, 160–167. https://doi.org/
10.1016/J.LWT.2018.01.037
Coelho, E., Magalhães, J., Pereira, F. B., Macieira, F., Domingues, L., & Oliveira, J. M.
(2019). Volatile fingerprinting differentiates diverse-aged craft beers. LWT, 108,
129–136. https://doi.org/10.1016/J.LWT.2019.03.044
Colicchio, T., Bamforth, C. W., Philliskirk, G., Villa, K., Stempfl, W., & Hayes, P. (2011).
In G. Oliver (Ed.), The oxford companion to beer. Oxford University Press. Oxford
University Press, Inc.
Cortese, M., Gigliobianco, M. R., Peregrina, D. V., Sagratini, G., Censi, R., & Di
Martino, P. (2020). Quantification of phenolic compounds in different types of crafts
beers, worts, starting and spent ingredients by liquid chromatography-tandem mass
spectrometry. Journal of Chromatography A, 1612, Article 460622. https://doi.org/
10.1016/j.chroma.2019.460622
Dantas, A., Quinteros, G. J., Darvishvand, S. Y., Blanco, M., Hernandez, E.,
Prudencio, E. S., et al. (2021). The combined use of progressive and block freeze
concentration in lactose-free milk: Effect of process parameters and influence on the
content of carbohydrates and proteins. Journal of Food Process Engineering, 44(11),
1–13. https://doi.org/10.1111/jfpe.13867
Depraetere, S. A., Delvaux, F., Coghe, S., & Delvaux, F. R. (2004). Wheat variety and
barley malt properties: Influence on haze intensity and foam stability of wheat beer.
Journal of the Institute of Brewing, 110(3), 200–206. https://doi.org/10.1002/J.2050-
0416.2004.TB00203.X
Eyres, G., & Dufour, J. P. (2008). Hop essential oil: Analysis, chemical composition and
odor characteristics. In Beer in health and disease prevention (pp. 239–254). Elsevier.
https://doi.org/10.1016/b978-0-12-373891-2.00022-5.
Fang, H., Wu, H. L., Wang, T., Chen, Y., Chang, Y. Y., Ding, Y. J., et al. (2022).
Authentication of craft and industrial beers by excitation-emission matrix
fluorescence spectroscopy and chemometrics. Microchemical Journal, 181(May),
Article 107650. https://doi.org/10.1016/j.microc.2022.107650
Gernat, D. C., Brouwer, E. R., Faber-Zirkzee, R. C., & Ottens, M. (2020). Flavour-
improved alcohol-free beer – quality traits, ageing and sensory perception. Food and
Bioproducts Processing, 123, 450–458. https://doi.org/10.1016/J.FBP.2020.07.014
Gernat, D. C., Penning, M. M., Swinkels, F. M., Brouwer, E. R., & Ottens, M. (2020).
Selective off-flavor reduction by adsorption: A case study in alcohol-free beer. Food
and Bioproducts Processing, 121, 91–104. https://doi.org/10.1016/j.fbp.2019.12.007
Gómez-Corona, C., Escalona-Buendía, H. B., García, M., Chollet, S., & Valentin, D.
(2016). Craft vs. industrial: Habits, attitudes and motivations towards beer
12
LWT 191 (2024) 115662
consumption in Mexico. Appetite, 96, 358–367. https://doi.org/10.1016/J.
APPET.2015.10.002
Gonzalez Viejo, C., Fuentes, S., Torrico, D. D., Godbole, A., & Dunshea, F. R. (2019).
Chemical characterization of aromas in beer and their effect on consumers liking.
Food Chemistry, 293, 479–485. https://doi.org/10.1016/j.foodchem.2019.04.114
Haas, I. C. da S., Espindola, J. S. de, de Liz, G. R., Luna, A. S., Bordignon-Luiz, M. T.,
Prudêncio, E. S., et al. (2022). Gravitational assisted three-stage block freeze
concentration process for producing enriched concentrated orange juice (Citrus
sinensis L.): Multi-elemental profiling and polyphenolic bioactives. Journal of Food
Engineering, 315, Article 110802. https://doi.org/10.1016/j.jfoodeng.2021.110802
Hills, E. E., Abraham, M. H., Hersey, A., & Bevan, C. D. (2011). Diffusion coefficients in
ethanol and in water at 298 K: Linear free energy relationships. Fluid Phase Equilibria,
303, 45–55. https://doi.org/10.1016/j.fluid.2011.01.002
ISO. (2006). ISO 5496:2006 Initiation and training of assessors in the detection and
recognition of odours. International Organization for Standardization. https://www.
iso.org/standard/44247.html.
ISO. (2011). International organization for standardization. ISO 3972:2011 Method of
investigating sensitivity of taste https://www.iso.org/standard/50110.html.
ISO. (2015). ISO 11035:1994 Sensory analysis — identification and selection of descriptors
for establishing a sensory profile by a multidimensional approach. International
Organization for Standardization. https://www.iso.org/standard/19015.html.
ISO. (2018). ISO 5667-3:2018 Determitation of solids content. International Organization
for Standardization. https://www.iso.org/standard/72370.html.
ISO. (2023). ISO 8586:2023 Selection and training of sensory assessors. International
Organization for Standardization. https://www.iso.org/standard/76667.html.
Jaeger, S. R., Worch, T., Phelps, T., Jin, D., & Cardello, A. V. (2020). Preference segments
among declared craft beer drinkers: Perceptual, attitudinal and behavioral responses
underlying craft-style vs. traditional-style flavor preferences. Food Quality and
Preference, 82. https://doi.org/10.1016/j.foodqual.2020.103884
Jiang, X., Wan, D., Zheng, F., & Xie, Y. (2022). Ionization equilibrium of water molecule
dominated ethanol-water binary solution self-assemble. Electrochemistry, 90(6).
https://doi.org/10.5796/ELECTROCHEMISTRY.22-00054
Khaireh, M. A., Angot, M., Cilindre, C., Liger-Belair, G., & Bonhommeau, D. A. (2021).
Article unveiling carbon dioxide and ethanol diffusion in carbonated water-ethanol
mixtures by molecular dynamics simulations. Molecules, 26(6). https://doi.org/
10.3390/molecules26061711
Kishimoto, T., Noba, S., Yako, N., Kobayashi, M., & Watanabe, T. (2018). Simulation of
Pilsner-type beer aroma using 76 odor-active compounds. Journal of Bioscience and
Bioengineering, 126(3), 330–338. https://doi.org/10.1016/j.jbiosc.2018.03.015
de Lima, A. C., Aceña, L., Mestres, M., & Boqué, R. (2023). Monitoring the evolution of
the aroma profile of lager beer in aluminium cans and glass bottles during the
natural ageing process by means of HS-spme/GC-MS and multivariate analysis.
Molecules, 28(6). https://doi.org/10.3390/molecules28062807
Li, F., Men, Z., Li, S., Wang, S., Li, Z., & Sun, C. (2018). Study of hydrogen bonding in
ethanol-water binary solutions by Raman spectroscopy. Spectrochimica Acta - Part A:
Molecular and Biomolecular Spectroscopy, 189, 621–624. https://doi.org/10.1016/j.
saa.2017.08.077
Lin, T., Quan, X., Cheng, P., Li, J., & Chen, G. (2020). Interaction between nanoparticles
and advancing ice-water interfaces: A molecular dynamics simulation. International
Journal of Heat and Mass Transfer, 163. https://doi.org/10.1016/j.
ijheatmasstransfer.2020.120412
Martins, C., Brandão, T., Almeida, A., & Rocha, S. M. (2018). Unveiling the lager beer
volatile terpenic compounds. Food Research International, 114, 199–207. https://doi.
org/10.1016/j.foodres.2018.07.048
Masuda, H., Ryuzaki, T., & Iyota, H. (2022). Role of agitation in the freezing process of
liquid foods using sucrose aqueous solution as a model liquid. Journal of Food
Engineering, 330. https://doi.org/10.1016/J.JFOODENG.2022.111100
Meneses, D. L., Ruiz, Y., Hernandez, E., & Moreno, F. L. (2021). Multi-stage block freeze-
concentration of green tea (Camellia sinensis) extract. Journal of Food Engineering,
293, Article 110381. https://doi.org/10.1016/j.jfoodeng.2020.110381
Miyawaki, O., & Inakuma, T. (2021). Development of progressive freeze concentration
and its application: A review. Food and Bioprocess Technology, 14(1), 39–51. https://
doi.org/10.1007/s11947-020-02517-7
Miyawaki, O., Omote, C., Gunathilake, M., Ishisaki, K., Miwa, S., Tagami, A., et al.
(2016). Integrated system of progressive freeze-concentration combined with partial
ice-melting for yield improvement. Journal of Food Engineering, 184, 38–43. https://
doi.org/10.1016/j.jfoodeng.2016.03.019
Moreno, F. L., Quintanilla-Carvajal, M. X., Sotelo, L. I., Osorio, C., Raventós, M.,
Hernández, E., et al. (2015). Volatile compounds, sensory quality and ice
morphology in falling-film and block freeze concentration of coffee extract. Journal
of Food Engineering, 166, 64–71. https://doi.org/10.1016/j.jfoodeng.2015.05.018
Moreno, F. L., Raventós, M., Hernández, E., & Ruiz, Y. (2014). Behaviour of falling-film
freeze concentration of coffee extract. Journal of Food Engineering, 141, 20–26.
https://doi.org/10.1016/j.jfoodeng.2014.05.012
Mosher, R. (2017). Tasting Beer: An insider’s guide to the World’s greatest drink. Storey
Publishing, LLC.
Moussaoui, C., Blanco, M., Muñoz, I. de B., Raventós, M., & Hernández, E. (2021). An
approach to the optimization of the progressive freeze concentration of sucrose
solutions in an agitated vessel. Separation Science and Technology, 56(4), 746–756.
https://doi.org/10.1080/01496395.2018.1508231
Muñoz, I. de B., Rubio, A., Blanco, M., Raventós, M., Hernández, E., & Prudêncio, E. S.
(2019). Progressive freeze concentration of skimmed milk in an agitated vessel:
Effect of the coolant temperature and stirring rate on process performance. Food
Science and Technology International, 25(2), 150–159. https://doi.org/10.1177/
1082013218803263
M. Osorio et al.
Nakagawa, K., Maebashi, S., & Maeda, K. (2009). Concentration of aqueous dye solution
by freezing and thawing. Canadian Journal of Chemical Engineering, 87(5), 779–787.
https://doi.org/10.1002/cjce.20213
Nakagawa, K., Nagahama, H., Maebashi, S., & Maeda, K. (2010). Usefulness of solute
elution from frozen matrix for freeze-concentration technique. Chemical Engineering
Research and Design, 88(5–6), 718–724. https://doi.org/10.1016/j.
cherd.2009.11.007
NIST Mass Spectrometry Data Center. (2006). NIST chemistry WebBook. Choice Reviews
Online, 43(12), 43Sup–293. https://doi.org/10.5860/choice.43sup-0293, 43Sup –
0293.
Olaniran, A. O., Hiralal, L., Mokoena, M. P., & Pillay, B. (2017). Flavour-active volatile
compounds in beer : Production , regulation and control. Journal of the Institute of
Brewing, 123(October 2016), 13–23. https://doi.org/10.1002/jib.389
Orellana-Palma, P., Lazo-Mercado, V., Gianelli, M. P., Hernández, E., Zúñiga, R. N., &
Petzold, G. (2020). Influence of cryoconcentration on quality attributes of apple
juice (Malus Domestica cv. Red Fuji). Applied Sciences (Switzerland), 10(3). https://
doi.org/10.3390/app10030959
Orellana-Palma, P., Petzold, G., Pierre, L., & Pensaben, J. M. (2017). Protection of
polyphenols in blueberry juice by vacuum-assisted block freeze concentration. Food
and Chemical Toxicology, 109, 1093–1102. https://doi.org/10.1016/j.
fct.2017.03.038
Orellana-Palma, P., Tobar-Bolaños, G., Casas-Forero, N., Zúñiga, R. N., & Petzold, G.
(2020). Quality attributes of cryoconcentrated calafate (berberis microphylla) juice
during refrigerated storage. Foods, 9(9), 1–19. https://doi.org/10.3390/
foods9091314
Osorio, M., Moreno, F. L., Hernández, E., & Ruiz-Pardo, R. Y. (2023). Impact of falling-
film freeze concentration in a commercial Lager beer. Journal of Food Process
Engineering. , Article e14292. https://doi.org/10.1111/JFPE.14292
Osorio, M., Moreno, F. L., Raventós, M., Hernández, E., & Ruiz, Y. (2018). Progressive
stirred freeze-concentration of ethanol-water solutions. Journal of Food Engineering,
224, 71–79. https://doi.org/10.1016/J.JFOODENG.2017.12.026
Palmioli, A., Alberici, D., Ciaramelli, C., & Airoldi, C. (2020). Metabolomic profiling of
beers: Combining 1H NMR spectroscopy and chemometric approaches to
discriminate craft and industrial products. Food Chemistry, 327(May), Article
127025. https://doi.org/10.1016/j.foodchem.2020.127025
Paszkot, J., Gasiński, A., & Kawa-Rygielska, J. (2023). Evaluation of volatile compound
profiles and sensory properties of dark and pale beers fermented by different strains
of brewing yeast. Scientific Reports, 13(1). https://doi.org/10.1038/s41598-023-
33246-4
Petzold, G., & Aguilera, J. M. (2009). Ice morphology: Fundamentals and technological
applications in foods. Food Biophysics, 4(4), 378–396. https://doi.org/10.1007/
s11483-009-9136-5
Petzold, G., Orellana, P., Moreno, J., Cerda, E., & Parra, P. (2016). Vacuum-assisted block
freeze concentration applied to wine. Innovative Food Science & Emerging
Technologies, 36, 330–335. https://doi.org/10.1016/J.IFSET.2016.07.019
Pieczonka, S. A., Hemmler, D., Moritz, F., Lucio, M., Zarnkow, M., Jacob, F., et al.
(2021). Hidden in its color: A molecular-level analysis of the beer’s maillard reaction
network. Food Chemistry, 361(March). https://doi.org/10.1016/j.
foodchem.2021.130112
Piggott, J. (2012). Alcoholic beverages Sensory evaluation and consumer research.
Woodhead Publishing Limited. Elsevier. https://www.sciencedirect.com/book/9780
857090515/alcoholic-beverages.
Preedy, V. R. (2008). Beer in health and disease prevention. Beer in Health and Disease
Prevention, 1–1101. https://doi.org/10.1016/B978-0-12-373891-2.X0001-6
Qin, D., Shen, Y., Yang, S., Zhang, G., Wang, D., Li, H., et al. (2022). Whether the
research on ethanol–water microstructure in traditional baijiu should Be
strengthened? Molecules, 1–14.
Ramos, F. A., Delgado, J. L., Bautista, E., Morales, A. L., & Duque, C. (2005). Changes in
volatiles with the application of progressive freeze-concentration to Andes berry
(Rubus glaucus Benth). Journal of Food Engineering, 69(3), 291–297. https://doi.org/
10.1016/j.jfoodeng.2004.07.022
Reinoso-Carvalho, F., Dakduk, S., Wagemans, J., & Spence, C. (2019). Dark vs. light
drinks: The influence of visual appearance on the consumer’s experience of beer.
Food Quality and Preference, 74, 21–29. https://doi.org/10.1016/j.
foodqual.2019.01.001
Saint-Michel, B., Georgelin, M., Deville, S., & Pocheau, A. (2017). Interaction of multiple
particles with a solidification front: From compacted particle layer to particle
trapping. Langmuir, 33(23), 5617–5627. https://doi.org/10.1021/acs.
langmuir.7b00472
Samsuri, S., Li, T. H., Ruslan, M. S. H., & Amran, N. A. (2020). Antioxidant recovery from
pomegranate peel waste by integrating maceration and freeze concentration
13
LWT 191 (2024) 115662
technology. International Journal of Food Engineering, 1. https://doi.org/10.1515/ijfe-
2019-0232 (ahead-of-print).
Sánchez, J., Ruiz, Y., Auleda, J. M., Hernandez, E., & Raventos, M. (2009). Review.
Freeze concentration in the fruit juices industry. Food Science and Technology
International, 15(4), 303–315. https://doi.org/10.1177/1082013209344267
Scarano, S., Pascale, E., Palladino, P., Fratini, E., & Minunni, M. (2018). Determination of
fermentable sugars in beer wort by gold nanoparticles@polydopamine: A layer-by-
layer approach for localized surface plasmon resonance measurements at fixed
wavelength. Talanta, 183, 24–32. https://doi.org/10.1016/j.talanta.2018.02.044
Sharp, D. C., Steensels, J., & Shellhammer, T. H. (2017). The effect of hopping regime,
cultivar and β-glucosidase activity on monoterpene alcohol concentrations in wort and
beer. https://doi.org/10.1002/jib.418
Sohrabvandi, S., Mortazavian, A. M. M., & Rezaei, K. (2012). Health-related aspects of
beer: A review. International Journal of Food Properties, 15(2), 350–373. https://doi.
org/10.1080/10942912.2010.487627
Strong, G. (2021). Beer judge certification program 2021 style guidelines. Beer Judge
Certification Program. https://www.bjcp.org/bjcp-style-guidelines/.
Tang, K., & Li, Q. (2017). Chapter 12: Beers. In Current developments in biotechnology and
bioengineering (pp. 306–307). Elsevier. https://doi.org/10.1016/B978-0-444-63664-
5.00001-0.
The Good Scents Company. (2018). The Good Scents Company information system. Www.
Thegoodscentscompany.Com/ https://www.thegoodscentscompany.com/.
Tian, J. (2010). Determination of several flavours in beer with headspace sampling–gas
chromatography. Food Chemistry, 123(4), 1318–1321. https://doi.org/10.1016/j.
foodchem.2010.06.013
Tyagi, S., Huynh, H., Monteux, C., & Deville, S. (2020). Objects interacting with
solidification fronts: Thermal and solute effects. Materialia, 12, 1–20. https://doi.
org/10.1016/j.mtla.2020.100802
Uald-Lamkaddam, I., Dadrasnia, A., Llenas, L., Ponsá, S., Colón, J., Vega, E., et al. (2021).
Application of freeze concentration technologies to valorize nutrient-rich effluents
generated from the anaerobic digestion of agro-industrial wastes. Sustainability, 13
(24), Article 13769. https://doi.org/10.3390/su132413769
Ueadaira, H., & Ueddaira, H. (1969). Diffusion coefficients of xylose in aqueous solution
maltose. Bulletin of the Chemical Society of Japan, 42(8), 2140–2142.
Uhlmann, D. R., Chalmers, B., & Jackson, K. A. (1964). Interaction between particles and
a solid-liquid interface. Journal of Applied Physics, 35(10), 2986–2993. https://doi.
org/10.1063/1.1713142
Van Doorn, G., Timora, J., Watson, S., Moore, C., & Spence, C. (2019). The visual
appearance of beer: A review concerning visually-determined expectations and their
consequences for perception. In Food research international (Vol. 126). https://doi.
org/10.1016/j.foodres.2019.108661
Verhagen, L. C. (2010). Beer flavor. In Comprehensive natural products II (pp. 967–997).
Elsevier. https://doi.org/10.1016/B978-008045382-8.00087-3.
Villacreces, S., Blanco, C. A., & Caballero, I. (2022). Developments and characteristics of
craft beer production processes. Food Bioscience, 45, Article 101495. https://doi.org/
10.1016/j.fbio.2021.101495
Vuist, J. E., Boom, R. M., & Schutyser, M. A. I. (2020). Solute inclusion and freezing rate
during progressive freeze concentration of sucrose and maltodextrin solutions.
Drying Technology, 1–9. https://doi.org/10.1080/07373937.2020.1742151
Vuist, J. E., Schutyser, M. A. I., & Boom, R. M. (2022). Solute inclusion during
progressive freeze concentration: A state diagram approach. Journal of Food
Engineering, 320, Article 110928. https://doi.org/10.1016/J.
JFOODENG.2021.110928
Wu, Y.-Y. Y., Xing, K., Zhang, X.-X. X., Wang, H., Wang, Y., Wang, F., et al. (2017).
Influence of freeze concentration technique on aromatic and phenolic compounds,
color attributes, and sensory properties of Cabernet Sauvignon wine. Molecules, 22
(6), 1–18. https://doi.org/10.3390/molecules22060899
Xu, C., Kolliopoulos, G., & Papangelakis, V. G. (2022). Industrial water recovery via layer
freeze concentration. Separation and Purification Technology, 292, Article 121029.
https://doi.org/10.1016/J.SEPPUR.2022.121029
Yang, N., Wu, C., Yang, H., Guo, Z., Jian, H., Jiang, T., et al. (2022). Bioactive
compounds, antioxidant activities and flavor volatiles of lager beer produced by
supplementing six jujube cultivars as adjuncts. Food Bioscience, 50, Article 102008.
https://doi.org/10.1016/J.FBIO.2022.102008
Yuan, G., Ren, J., Ouyang, X., Wang, L., Wang, M., Shen, X., et al. (2016). Effect of raw
material, pressing and glycosidase on the volatile compound composition of wine
made from goji berries. Molecules, 21(10). https://doi.org/10.3390/
molecules21101324
Zhang, L., Wang, Q., Liu, Y. C., & Zhang, L. Z. (2006). On the mutual diffusion properties
of ethanol-water mixtures. Journal of Chemical Physics, 125(10). https://doi.org/
10.1063/1.2244547