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Food Research International

journal homepage: www.elsevier.com/locate/foodres

Chemical and sensory evaluation of cold brew coffees using different

roasting profiles and brewing methods
Nancy Córdoba a, Fabian L. Moreno b, Coralia Osorio c, Sebastián Velásquez d, Yolanda Ruiz b, *
a
Doctoral Program in Biosciences, Faculty of Engineering, Universidad de La Sabana, Campus Universitario Puente del Común, Km. 7 Autopista Norte, Bogotá 25001,
Colombia
b
Grupo de Investigación en Procesos Agroindustriales, Universidad de La Sabana, Campus Universitario Puente del Común, Km. 7 Autopista Norte, Bogotá 25001,
Colombia
c
Departamento de Química, Universidad Nacional de Colombia-Sede Bogotá, AA 14490 Bogotá, Colombia
d
Research & Development Department, Industria Colombiana de Café, Medellín, Antioquia, Colombia

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

Keywords: This study evaluated the effects of different roasting profiles (time/temperature) and brewing methods on the
Coffee roasting physicochemical and sensory characteristics of coffee brews. Cold brewing (dripping and immersion) and hot
Extraction brewing (French press) methods were studied to understand the effects of water temperature and technical
Volatile compounds
brewing method conditions on the chemical compound extraction in coffees roasted at high-temperature short
Caffeoylquinic acids
time (HTST) and low-temperature long time (LTLT). The results showed that coffee beverages were clearly
Caffeine
Sensory profile differentiated concerning the roasting profile when hot water was used (90 ± 3 ◦ C) in brewing. Separation of
beverages according to the water temperature used in brewing was observed. Notably, hot brewing coffees were
distinguished from cold brewing (19 ± 2 ◦ C) based on a higher titratable acidity and abundance of some furan
compounds. The non-volatile extraction rate increased at higher brewing temperatures. At the same brewing
temperature, dripping exhibited a higher extraction rate than immersion brewing, which suggests that the coffee
extraction process is affected by the design and operation of the cold brewing system. Coffee beverages brewed
with HTST and cold dripping displayed the highest value in total dissolved solids (TDS), extraction yield, as well
as the highest caffeine, trigonelline, 4- and 5-caffeoylquinic acids (CQAs) contents. Regardless of the roasting
profile, coffees brewed by cold dripping were perceived with more bitter and roasted flavors. In contrast, cold
immersion and hot coffee beverages showed remarkable sweetness, nutty, caramel, and malt attributes. In turn,
these attributes showed an inverse correlation with caffeine concentration, trigonelline, CQAs, and TDS. The
findings of this study demonstrate that volatile and non-volatile compounds present in roasted coffee depend on
time-temperature roasting conditions; in turn, their presence in the resulting beverages are related to the
extraction of the operational conditions of coffee brewing methods.

1. Introduction significantly contribute to the perceived sensory characteristics of the

Coffee brewing is a solid-liquid extraction wherein the process pa-
rameters have a significant impact on the extraction kinetics of the
different chemical compounds present in roasted coffee (Cordoba,
Fernandez-Alduenda, Moreno, & Ruiz, 2020). Volatile and non-volatile
chemical compounds are produced via Maillard pyrolysis and Strecker
degradation reactions upon roasting (Seninde & Chambers, 2020).
During extraction, soluble and non-soluble compounds are dissolved in
the extraction water and depending on the extraction technique. These
compounds end up in the extract as dissolved or suspended solids that
coffee brew (Sánchez-López, Wellinger, Gloess, Zimmermann, & Yer-
etzian, 201 ).
Consumers usually prefer high-quality and healthy beverages; this
leads to the increasing demands for the production of coffee brews with
high and unique sensory characteristics (Barbosa, Scholz, itzberger, &
Benassi, 2019). Within these trends, cold brew coffee has become one of
the most popular drinks in specialty coffee shops around the world
(Grant, 2020). Market analysis shows that the market for cold brew
coffee was valued at S 321 million in 201 , and it is expected to reach
S 1.3 billion by 2023 (Shahbandeh, 2020).

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

https //doi.org/10.101 / .foodres.2021.110141

Received 25 August 2020; Received in revised form 5 anuary 2021; Accepted 5 anuary 2021
N. Córdoba et al.
Cold brew coffee is obtained via extraction of water at 20–25 ◦ C or at
lower temperatures, and over a longer period that can vary from to 24
h (Cordoba, ataquiva, Osorio, Moreno, & Ruiz, 2019; Fuller & Rao,
201 ). Cold brew coffee is often made by dripping and immersion
methods. These systems for cold brewing differ in several technical as-
pects, including the configuration of the coffee beds and the required
brewing time. The cold dripping system allows continuous renewal of
water. Contrastingly, in cold immersion systems, the coffee remains
inside filter bags in a static system and directly immersed in the aqueous
solution. Cold brew coffee has been reported to possess a different flavor
profile, which is typically characterized by intense sweetness, chocolate,
fruity and floral odor-notes, medium bitterness and acidity, and a
creamy body, as the extraction conditions (time/temperature) differ
from those in traditional hot coffee brewing (Angeloni, Guerrini,
Masella, Innocenti, et al., 2019; Cordoba et al., 2019). Although cold
brew coffee is a growing widespread trend in the coffee market (Mar-
ketersMedia, 2020), information that supports their remarkable differ-
ences and distinctive characteristics compared with hot coffee brew is
limited. Several recent reports have focused on studying the cold coffee
extraction process. Non-volatile compounds, such as caffeine, trigonel-
line, and caffeoylquinic acids (CQAs), have been the most studied
compounds in cold brew coffee (Angeloni, Guerrini, Masella, Bellumori,
et al., 2019; Angeloni, Guerrini, Masella, Innocenti, et al., 2019; Fuller &
Rao, 201 ; Rao & Fuller, 201 ; Rao, Fuller, & Grim, 2020).
CQAs and caffeine concentrations in cold brew coffees have shown
associations with the degree of roasting and water temperature used
during the extraction process (Fuller & Rao, 201 ). Compared to hot
brew coffees, cold brews show decreased acidity, lower concentration of
browned compounds, and fewer total dissolved solids (TDS), indicating
that cold water brewing extracts certain compounds less effectively than
hot water brewing (Rao et al., 2020). Although coffees at different de-
grees of roasting have been studied, to the best of the authors’ knowl-
edge, the effect of roast profiles (time/temperature) on the preparation
of cold beverages has not been addressed yet. In the roasting process, the
chemical reactions that occur during the process depend on heat
transfer. Therefore, the balance between time and temperature to reach
a certain color degree during this process directly affects the final
chemical composition and sensory properties of the coffee brews (Toci,
Azevedo, & Farah, 2020).
Volatile organic compounds (VOCs) have been widely reported in
roasted coffee and hot coffee brews. However, published reports for cold
brew coffees are scarce. Some flavor compounds such as 2-furfuryl ac-
etate, 5-methyl furfural, pyridine, furfural, 2-acetyl furan, pyridine, 2-
methoxy phenol, and furfuryl alcohol were identified in cold brew ex-
tracts obtained by dripping (Hwang, im, ang, im, & im, 2014).
Additionally, the presence of some furans, pyrazines, ketones, alde-
hydes, pyrroles, esters, lactones, furanones, and phenols were reported
in cold brew coffee prepared at 19 ◦ C with specialty coffee from
Colombia (Cordoba et al., 2019).
The chemical and sensory characteristics of coffee brews are asso-
ciated with the non-volatile and volatile compositions of roasted coffee.
These characteristics are known to be developed during the roasting
process (Gloess et al., 2014). Recent studies have observed that the
degree of roasting, coffee to water ratio, brewing method (BM), and
their interactions affect the sensory characteristics of cold brew coffees
(Seninde, Chambers, & Chambers, 2020). In addition, cold drip coffees
have been described as more bitter than cold brews made by the im-
mersion method (Angeloni, Guerrini, Masella, Innocenti, et al., 2019).
Several extraction variables have been widely studied in hot brew-
ing. In contrast, in cold extraction, only a few studies regarding the ef-
fect of several extraction variables on the chemical and sensory
characteristics of coffee brews have been conducted. Hence, the present
study aimed to evaluate the impact of the roasting profile (R ) (time-
temperature) and the BM on the physicochemical and sensory charac-
teristics of coffee brews. Cold brewing (dripping and immersion) and an
example of conventional hot brewing (French press) methods were
studied to better understand the role of water temperature and the
technical BM conditions on the extraction of the chemical compounds
present in the roasted coffees.
2. Material and methods
2.1. Chemicals and reagents
Caffeine, trigonelline, 5-caffeoylquinic acid, 4-caffeoylquinic acid
standards, Acetic acid, and methanol were from Sigma-Aldrich (St.
Louis, MO, SA). A mixture of n-alkanes (C –C2 ) was purchased from
Laboratory Dr. Ehrenstorfer GmbH (Augsburg, Germany).
2.2. Coffee samples
Specialty Arabica coffee (Coffea arabica) from Linares-Nariño
(Colombia) was used in all experiments. Green coffee beans were pro-
cessed by smallholder coffee growers in 201 and roasted according to
the methodology described in section 2.3. Roasted coffees were ground
in a commercial mill (B NN , Mexico D.F.) until coarse grinding
( 01–900 μm). Grinding level was determined according to the
Colombian National Standard NTC 2441 (ICONTEC, 2011).
2.3. Coffee roasting
Batches of 2 kg of green coffee beans were roasted using a Samiac
drum roaster with heating propane gas (Sasa Saminac, GE10/12,
France). Coffee samples were roasted until the two different R s, high-
temperature short time (HTST) and low-temperature long time (LTLT)
to a medium roast degree were achieved; R s were achieved by
ad usting heat intensity through regulating air flow. The time-
temperature profiles used for the experiments are shown in Fig. 1.
Roasting parameters were monitored using Cropster Roasting (Crop-
ster , Austria). At the end of the roasting process, each batch was cooled
down with an air inlet supplied by the roasting machine. Colour CIELAB
parameters were measured and expressed in L*(Lightness), a* (redness/
greenness), and b* (yellowness/blueness) coordinates ( onica Minolta
Sensing Americas Inc, Ramsey, N , SA). The roasting parameters fol-
lowed by the roast batches are mentioned in Table 1. All roasting pro-
files were made in duplicate. Roasted beans were stored until coffee
brewing in 2.5 kg golden bags ( ET/AL/ EBD/VALVE, Sellopack ,
Colombia) at − 20 ◦ C.
2.4. Coffee BM
Cold brew coffee samples were prepared by dripping (CD) and im-
mersion (CI). The operating variables of the coffee BM were ad usted
according to preliminary studies (Angeloni et al., 2019; Cordoba,
ataquiva, Osorio, Moreno, & Ruiz, 2019), with some modifications.
Cold drip coffees were prepared using Cold Bruer equipment (Bruer,
Santa Cruz, California, SA). The flow water average was fixed in 9.0 ±
1.0 drops every 30 s, for an average extraction time of .5 h. For cold
immersion brews, coffee grounds were placed into a filter bag and
submerged into the water in steeping conditions for 14 h. For both
methods, 31.5 g of ground coffee and 350 mL of filtered water were
used. Cold extraction for both methods was carried out at 19 ± 2 ◦ C. The
French ress system (Bodum , Inc., NY, SA) was used for hot brewing
(HB). Filtered hot water (250 mL, 90 ± 3 ◦ C) was poured over the ground
coffee (22.5 g) placed in the French press glass. After 5 min, the plunger
was pressed over the coffee grounds until it reached the bottom of the
vessel.
2.5. Chemical characterization of the coffee samples
2.5.1. TDS and extraction yield (EY)
TDS was measured according to a previously described methodology
N. Córdoba et al.

Fig. 1. Models of time–temperature roasting profile used in the experiments. Data shows mean and standard deviation of data for roasting profiles. HTST High -
Temperature Short Time; LTLT Low - Temperature long time. All the experiments were made in duplicate to reach medium roast degree.

diode array detector ( DA). The separation was achieved in a Gemini

Table 1
column C-1 ( henomenex, SA; 250 mm × 4. mm i.d., 5 μm) at 25 ◦ C.
arameters for time-temperature roasting profiles of the coffee roasted batches
The mobile phase used was acetic acid 1 (A) and methanol (B). The
used in the coffee extraction.
gradient was ad usted as follows 0– min A/B 9 /4; 20 min A/B 2/
Parameters HTST LTLT 2 ; 25–2 min, A/B 5 /42 at a flow rate of 1.5 mL min−1. CQAs were
Weight loss (%) 15.39 ± 0. 1 .22 ± 0.11 detected at λ 325 nm, and caffeine and trigonelline at λ 2 5 nm. The
Initial temperature (◦ C) 21 .45 ± 0.50 140.45 ± 2.00 in ection volume was 10 μL. The non-volatile compounds were quanti-
End Temperature (◦ C) 195.40 ± 2.00 1 4.30 ± 0. 0
tated by using the external standard method in the H LC- DA equip-
Roasting time (min) 5.32 ± 0.00 15. ± 0. 0
L* 29. 4 ± 0.42 2 .30 ± 139 ment. Concentrations were calculated using the regression equation
a* 14.05 ± 0.22 13. ± 0.19 with good linearity (R2 > 0.994) of the external standards. All samples
b* 23.21 ± 0.30 22.4 ± 0.52 were analyzed in triplicate.
HTST (High-Temperature Short Time), and LTLT (Low-Temperature Long Time)
to medium roast degree. All experiments and measurements were performed in 2.5.4. VOC analysis
duplicate. The mean and SD (standard deviation) for each experimental Coffee samples were analyzed in triplicate directly after brewing
parameter is reported. using headspace solid-phase microextraction (HS-S ME) and gas chro-
matography/mass spectrometry (GC–MS) analyses. GC–MS analyses
(Gloess et al., 2013). EY was calculated as the product of TDS and the were done in a 59 A mass selective detector (Agilent Technologies Inc.,
total weight of water mass (Ww) divided by the ground coffee weight Wilmington, DE, SA) coupled to the Agilent 90B gas chromatograph,
used for the extraction (Wgc) (i.e., EY = (TDS * Ww/ Wgc)). in electron impact ionization mode at 0 eV. Mass spectra were recorded
in the range of 30–350 u. Each sample (2 g) was equilibrated for 1 h in a
2.5.2. pH and total titratable acidity (TA) 20 mL sealed vial at 1 ◦ C using a magnetic stirrer. The volatile com-
The pH value of the coffee samples was measured at 19 ± 2 ◦ C using a pounds released from the headspace of each sample were collected using
pH meter (Fisher Scientific, Ottawa, Canada). For TA, 50 mL of the an S ME fiber of poly-dimethylsiloxane/divinylbenzen ( DMS/DVB)
coffee extract was titrated with 0.1 mol / L NaOH solution to a pH of .5. with a 5-µm thick film (Supelco Inc., Bellefonte, A, SA) for 1 h at
The results were expressed in milligrams of chlorogenic acids per gram 1 ◦ C with agitation. Samples were then directly in ected into a gas
of coffee (mg CGA / g) according to the Colombian National Standard chromatograph 90B (Agilent Technologies Inc., Wilmington, DE,
NTC 524 (ICONTEC, 2004). SA) coupled to a 59 A mass selective detector (Agilent Technologies
Inc., Wilmington, DE, SA). A DB-FFA column (Agilent Technologies
2.5.3. Non-volatiles compounds analysis Inc., Wilmington, DE, SA, 50 m × 0.25 mm i.d., 0.32 μm) was used. The
The content levels of caffeine, trigonelline, and caffeoylquinic acids column oven was programmed from 45 (after 2 min) to 250 ◦ C at a rate
(CQAs, 4- and 5-caffeoylquinic) were determined by reversed-phase of 5 ◦ C / min, and the final temperature was maintained for 5 min. The
high-performance liquid chromatography (R -H LC), according to the in ector temperature was maintained at 250 ◦ C, the carrier gas He at 1.5
study of Moreno, Raventós, Hernández, & Ruiz (2014). Quantitative mL/min. Identification of the volatile compounds was performed by
analyses were carried out using a LaChrom H LC (Merck-Hitachi, Ger- comparing their mass spectra and retention indexes (retention index
many), equipped with a quaternary pump, degasification system, and a calculated by comparison with the retention times of C –C2 alkane
N. Córdoba et al.

standard mix) with the NIST mass spectra library (ver. 2.2, NIST/E A/ Table 2
NIH, 2014). Data were processed by the Class 5000 v 2.2 MS- Reference list and their definition used in the descriptive analysis of brewed
Workstation software. The average relative content of the VOCs was coffee.
calculated based on the percentage of the normalized peak area of the Category Specific Definition Reference
total ion current chromatogram. attributes

Basic taste Sweetness A fundamental taste 1.0 sucrose

2. . Sensory evaluation factor of which solution(a)
sucrose is typical (a)
Acidity The fundamental 0,015–0,05 Citric
The panel was included cuppers of Colombian specialty coffee
taste factor solution(a)
exporter companies, local specialty coffee stores, and researchers from associated with a
the food science and technology department of niversidad de La citric acid solution (a)
Sabana (Bogota-Colombia). The panel comprised eight volunteers (1 Bitterness The fundamental 0,01–0,04–0,05
female and males; age range 21–50 years for both genders), with more taste factor Caffeine solution(a)
associated with a
than 3 years of experience in the area of coffee sensory analysis. All caffeine solution(a)
experiments followed the relevant guidelines and regulations of ni- Aroma Nutty (AR,F) A slightly sweet, Hazelnut coffee flavor
versidad de La Sabana. The Research Commission of the Faculty of En- (AR) and brown, woody, oily, map ref. 040. uree
gineering of niversidad de La Sabana approved the procedures and Flavor musty, astringent, the almonds and
(F) and bitter aromatic walnuts separately(a)
methodologies. All panelists had provided informed consent. The
commonly associated
method for identifying and selecting descriptors was carried out ac- with nuts, seeds,
cording to the Colombian National Standard NTC 3932 (ICONTEC, beans, and grains(a)
199 ) and ISO 11035 (International Organization for Standardization Caramel (AR,F) A round, full-bodied, Caramel coffee flavor
(ISO), 1994). medium brown, map ref. 051
sweet aromatic
The assessors participated in two sessions (4 h each one) to develop a associated with
sensory vocabulary using different cold brew coffee preparations. A list cooked sugars and
of 25 descriptors was chosen and used in the sensory analysis (Table 2). other
All panelists were trained in each attribute selected according to the carbohydrates(a)
Chocolate (AR, A blend of cocoa, Dark chocolate coffee
coffee lexicon (Chambers et al., 201 ; World Coffee Research, 201 ). For
F) including cocoa flavor map ref. 05 .
the coffee samples analysis, a blind sensory descriptive analysis was butter and dark roast Chop dark chocolate
used. All samples were presented in a randomized order and served at aromatics at varying
19 ◦ C in clear glasses with an effective volume of 120 mL. Samples were intensities(a).
tested in duplicate, and three glasses for each sample were served. They Fruity (AR,F) A sweet, floral, uice kiwi strawberry
aromatic blend of a (100 ) (a). Strawberry
were analyzed immediately after the completion of the extraction time, variety of ripe coffee flavor map ref.
and they were covered with a glass lid until they were tasted. fruits(a). 015
First, global attributes (aroma, flavor, aftertaste, body, astringency, Malt (AR,F) The light brown, Beverage of malt. Malt
and balance) and basic taste (sweetness, acidity, and bitterness) in- dusty, musty, sweet, coffee flavor map ref.
sour and or slightly 04
tensities were evaluated. Following this, assessors evaluated the in-
fermented aromatic
tensity of each specific attribute. Assessors scored the intensity of each associated with
global attribute (Table 2) on a scale from 0 to 15 (0 = none, 2 = barely grains(a)
detectable, = slightly intense, = moderately intense, 10 = intense, Honey (AR, F) Sweet, light brown, Honey in water(a).
12–15 = very intense) (World Coffee Research, 201 ). slightly spicy Honey coffee flavor
aromatic associated map ref. 053
with honey(a).
2.7. Data analysis Non-centrifugal Sweet, dark, Local grated non-
cane sugar caramelized, centrifugal cane sugar
All data analyses were performed using R, version 3. .3, “Holding “ anela” (AR, F) aromatic impression
characterized for
the Windsock,” and LSTAT statistical software (Addinsoft, New York,
some sulfur notes
NY, SA). The Statistical significance was set at α = 0.05 for compari- similar to molasses.
sons was considered. A two-way fixed-effect ANOVA model, with the Roasted (AR, F) Dark brown Roasted coffee flavor
main effects of R , BM, and their interactions, was applied. Further- impression map ref. 050
more, Tukey pairwise comparisons were computed to evaluate the dif- characteristic of
products cooked to a
ference among the treatments. ruskal-Wallis and Dunn tests were used high temperature by
to compare the non-volatile rates among treatments. In the case of the dry heat(a)
sensory analysis, a mixed-effect model was considered. The panelists Vanilla (AR, F) A woody, slightly Vanilla Coffee flavor
were considered a random effect, and the variance explained by the chemical aromatic map ref. 0
associated with
random effect checked for each variable.
vanilla bean, which
Additionally, the random effect was considered for both the intercept may include brown,
and slope to compensate for the impact of possible bias induced by each beany, floral, and
panelist. For principal component analysis ( CA), all parameters phys- spicy notes(a)
icochemical and non-volatile concentration, as well as significant vola- Coffee ID (AR, F) A distinctly roasted Dark roasted coffee
brown, slightly bitter
tile and sensory data, were included. All variables were mean-centered aromatic
and scaled before analysis. characteristic of
brewed coffee(b)
3. Results and discussion Floral (F) A sweet, light, Rose coffee flavor map
slightly fragrant ref. 0
aromatic associated
3.1. Effect of RP with fresh flowers(a)
(continued on next page)
The main effect of the R was significant (p < 0.05) for 5-and 4-CQA
N. Córdoba et al.

Table 2 (continued ) and all physicochemical characteristics evaluated. High TDS, EY, 5-and
Category Specific Definition Reference 4-CQA concentration values (mg/mL) and a lower pH were detected in
attributes coffee roasted at HTST. The first four aforementioned variables exhibi-
Spices (F) The sweet, brown Cinnamon sticks and
ted a significant decrease when the R changed to LTLT, while pH
aromatic associated pulverized(a). increased (Table 3). Similar results regarding an increase in pH and a
with spices such as Cinnamon coffee decrease in chlorogenic acids in hot infusions brewed with coffees
cinnamon, clove, flavor map ref. 0 roasted at different roasting times ( , 9, and 11 min at 220 ± 10 ◦ C) have
nutmeg, and
been observed (Bicho, Leitão, Ramalho, de Alvarenga, & Lidon, 2013).
allspice(a).
Cereal (F) The light brown, Rice coffee flavor map In agreement with our results, previous studies have also shown that fast
dusty, musty, sweet ref. 049 roasting conditions (2.5–3.0 min) allow a smaller degradation of
aromatic associated chlorogenic acid; therefore, a shorter roasting time permits more
with grains(a) chlorogenic acid to remain in the bean (Nagara u, Murthy, Ram-
Woody (F) The sweet, brown, ine coffee flavor map
musty, dark aromatic ref. 0 2
alakshmi, & Srinivasa Rao, 199 ).
associated with a During the roasting process, the physical properties of coffee beans
bark of a tree(a) are strongly dependent on the applied temperature and roasting time
Green/ An aromatic Fresh parsley in (Baggenstoss, oisson, aegi, erren, & Escher, 200 ). High roasting
vegetative (F) characteristic of water(a)
temperature (e.g., HTST) affects the porosity and volume of coffee beans
fresh, plant-based
material. Attributes compared to low-temperature roasted beans (e.g., LTLT) (Schenker,
may include leafy, Handschin, Frey, erren, & Escher, 2000). These microstructural
unripe, grassy, and changes generated by the intense heat of roasting make compounds
peapod(a). more readily extractable (Rao et al., 2020). These phenomena could
Mouthfeel Body M Tactile feeling of the Samples of hot coffee
liquid in the mouth, prepared with roasted
explain the significantly higher TDS and extraction efficiency (mg/g
especially as coffees from different ground coffee) of CQAs when the HTST profile was used (Table 3-IIB).
perceived between origins. Likewise, changes in the coffee matrix can favor the extraction of other
the tongue and roof compounds such as organic acids or acidic components present in the
of the mouth (c)
roasted bean, which can explain the trend of superior TA in beverages
Astringency M A drying, puckering 0.05 Alum solution(a)
or tingling sensation, prepared with HTST coffees (Table 3-I). A ma or fraction of the acidity
on the surface and/or generated on coffee roasting can be attributed to the formation of four
edge of the tongue aliphatic acids formic, acetic, glycolic, and lactic during the roasting
and mouth(a). process (Azeredo, 2011). However, some of them can be degraded
General Aroma The smell of the Samples of hot coffee
depending on the roasting conditions (Ginz, Balzer, Bradbury, & Maier,
impact coffee beverage and cold brew coffee
generated by sniffing 2000).
aromas released of Regarding volatile composition, the R affected the total abundance
the cup of coffee. of pyrazines (p = 0.000), phenols (p = 0.005) and, furanones (p =
Flavor It is a combined Samples of hot coffee
0.00 ). These volatiles show a higher abundance in coffee brewed with
impression of all the and cold brew coffee
gustatory (taste bud) the HTST profile (Table 4). Likewise, the levels of five 2-ethyl-3-
sensations and retro- methylpyrazine (p = 0.020), 2,3-dimethyl-pyrazine (p = 0.040), ethyl-
nasal aromas that go pyrazine (p = 0.000), 2, -dimethylpyrazine (p = 0.000), and methyl-
from the mouth to pyrazine (p = 0.00) of the eight pyrazines detected were affected by
nose (c).
the R . Most of the contents of these pyrazines showed an increase in
Aftertaste Length of positive Samples of hot coffee
flavor qualities and cold brew coffee fast roasting (HTST) and tended to decrease the abundance with a longer
emanating from the roasting time (LTLT). Earlier studies have indicated that pyrazines are
back of the palate and significantly higher in fast roasting (4 min), and the abundance of pyr-
remaining after the
azine decrease with increasing roasting time until 15 min ( etisca,
coffee is expectorated
or swallowed(c)
érez- alacios, Farah, inho, & Ferreira, 2013). The presence of some
Balance How all the various Samples of hot coffee pyrazines such as 2-ethyl-2,5-dimethylpyrazine, exhibit a rapid increase
aspects of flavor, and cold brew coffee at the beginning of the roasting process, while those in over-roasted
aftertaste, acidity, coffees can be degraded (Baggenstoss et al., 200 ). Alkylpyrazines, as
and body of the
detected in the present work for cold and hot coffee brews, are consid-
sample work together
and complement or ered important coffee aroma compounds. Some specific pyrazines such
contrast to each as ethylpyrazine and 2-ethyl- -methylpyrazine, have also been found in
other(c). beverages such as espresso coffee, and these pyrazines have been asso-
Global Overall The maximum Samples of hot coffee
ciated with woody/papery and earthy/musty flavor notes, thereby
score overall sensory and cold brew coffee
impression(a). It
producing the remarkable coffee aroma (Maeztu et al., 2001).
reflects the Among phenols, the presence of 4-ethenyl-2-methoxyphenol (2-
holistically methoxy-4-vinylphenol) (p = 0.003) and phenol (p = 0.01 ) were sig-
integrated rating of nificant. 2-methoxy-4-vinylphenol has been reported as a key flavor
the sample as
compound associated with spicy and clove-like attributes (Amanpour &
perceived by the
individual panelist(c) Selli, 201 ). 2-methoxy-4-vinylphenol showed a trend toward higher
(a)
abundance at HTST, which decreased in LTLT R s. This behavior could
(World Coffee Research, 201 )
(b) be related to the dependence in the formation of 2-methoxy-4-vinylphe-
(Sanchez & Chambers, 2015)
(c) nol with the roasting process conditions. Due to thermal instability, once
(SCA, 2015).
4-vinylguaiacol reaches maximum concentration, it decreases over the
roasting time (Zimmermann, Heger, Yeretzian, Nagel, & Boesl, 199 ).
Regarding total furanones, a higher abundance was detected in
coffee brewed with the LTLT profile. In the present investigation, the
N. Córdoba et al.

Table 3
hysicochemical characteristics and non-volatile composition of coffee brewed at different roasting profile and brewing method.
Brewing method (BM) Cold dripping Cold immersion Hot brewing (French press) Individual factors and
interactions

Roasting profile (RP) HTST LTLT HTST LTLT HTST LTLT RP BM RP:
BM
(mean ± SD) p-value

I. Physicochemical characteristics
Total dissolved solids ( ) 2.01 ± 0.10a 2.03 ± 0.0 a 1.91 ± 0.04ab 1. ± 0.0 bc
1. 1 ± 0.14abc 1.55 ± 0.05c 0.015 0.001 NS
Extraction Yield ( ) 20. ± 1.01a 20. 3 ± 0. 4a 19. ± 1 .2 ± 1 .5 ± 15.93 ± 0.015 0.002 NS
0.49ab 0. 5bc 1.02abc 0.5 c
Titratable acidity (mg chlorogenic 4.54 ± 0.11ab 4.09 ± 0.19bc 4.21 ± 0.09bc 3. ± 0.1 c
4.91 ± 0.0 a 4. 2 ± 0.0 ab 0.001 0.000 NS
acids/g)
pH 4. ± 0.01ab 4. 0 ± 0.01a 4. 5 ± 0.02ab 4. 9 ± 0.02a 4. 0 ± 0.03b 4. 3 ± 0.01ab 0.022 0.009 NS

II.Non-volatile compounds
(II-A) Concentration (mg / mL)
Caffeine 1.42 ± 0.0 a 1.33 ± 0.11a 1.00 ± 0.05b 0.94 ± 0.05bc 0. 2 ± 0.04bc 0. 0 ± 0.04c NS 0.000 NS
Trigonelline 0. ± 0.03a 0. 5 ± 0.04a 0.5 ± 0.04b 0.53 ± 0.02bc 0.4 ± 0.02bc 0.4 ± 0.02c NS 0.000 NS
5-CQA 0. ± 0.0 a 0. 9 ± 0.05a 0.54 ± 0.03b 04 ± 0.02bc 0.43 ± 0.02c 0.39 ± 0.03c 0.004 0.000 NS
4-CQA 0.4 ± 0.03a 0.42 ± 0.03a 0.35 ± 0.02b 0.30 ± 0.01bc 0.2 ± 0.01 cd 0.24 ± 0.02d 0.002 0.000 NS

(II-B) Extraction efficiency (mg / g coffee ground)

Caffeine 14. ± 0. 5a 13. 1 ± 1.02a 10.2 ± 0.54b 9. ± 0.41bc .21 ± 0.42c .0 ± 0.42c NS 0.000 NS
Trigonelline ,01 ± 0.34a . 9 ± 0.41a 5, 5 ± 0.44b 5.51 ± 2.10bc 4. 5 ± 0.22 cd 4. 5 ± 0.1 d NS 0.000 NS
5-CQA .0 ± 0. 1a .1 ± 0.43a 5.5 ± 0.2 b 5.00 ± 0.20bc 4.29 ± 0.1 cd 3.9 ± 0.32d 0.005 0.000 NS
4-CQA 4.9 ± 0.33a 4.3 ± 0.2 a 3.5 ± 0.20b 3.15 ± 0.13bc 2. 0 ± 0. 0 cd 2,45 ± 0.20d 0.002 0.000 NS

(II-C) Intake per cup (mg / 100 mL)

Caffeine 142.03 ± 133.15 ± 99.54 ± 5.01b 94.35 ± 1. 9 ± 3. 1bc 9.90 ± NS 0.000 NS
.15a . 5a 4. 2bc 4.39c
a
Trigonelline . 4 ± 3.0 4.50 ± 4.43a 55. 3 ± 4.1 b
53.23 ± 4 .30 ± 1.9 bc
4 .03 ± NS 0.000 NS
2.10bc 1. 1c
5-CQA .02 ± 5.92a 9.12 ± 4. a
54.1 ± 2.5 b
4 .21 ± 42. ± 1.55c 39.19 ± 0.004 0.000 NS
2.23bc 3.32c
4-CQA 4 .1 ± 3.20a 42.25 ± 2. a
34.4 ± 1.91b 30.39 ± 2 . ± 1.1 24.24 ± 0.002 0.000 NS
1.4 bc cd
2.0 d

The means ± standard deviation (n = 3) and p-values for each two variables and their interactions, are reported. Different letters on the same raw means that the data
are significantly different (p < 0.05). NS, not significant effects (p > 0.05). R Roasting rofile, BM Brewing Method, R BM Roasting profile Brewing method
interaction, CD Cold dripping, CI Cold immersion, HB Hot brewing, HTST (High-temperature short time), LTLT (Low-temperature long time), 5-CQA 5-Caffeoyl-
quinic acid, 4-CQA 4- caffeoylquinic acid. (II-A) Content of different coffee brews. (II-B) Extraction efficiency, considering the amount of ground coffee used. (II-C)
Values were calculated considering one average volume for a coffee cup equal to 100 mL.

LTLT conditions used did not exceed 240 ◦ C and 15 min, our results are
in agreement with previous studies in which a high concentration of
furanones has been found under mild roasting conditions (240 ◦ C / 14
min), which tended to decrease when a higher roasting intensity (250 ◦ C
/ 20 min) was applied (Moon & Shibamoto, 2009). The furanones pro-
duce positive caramel/sweet and buttery odor notes (Toci & Boldrin,
201 ).
Other specific volatile compounds were also affected by the R s. For
instance, furan-2-yl-methyl acetate (furfurylacetate) (p = 0.030), 1-
methylpyrrole-2-carbaldehyde (p = 0.002), and 1H-pyrrole-2-carbal-
dehyde (p = 0.025) exhibited a trend toward higher abundance in cof-
fees brewed with the LTLT profile. yrroles are formed via Maillard
reaction, and previous studies have demonstrated that its formation is
affected by roasting intensities (Baggenstoss et al., 200 ; Moon & Shi-
bamoto, 2009). yrrole compounds have been associated with a
caramel-like buttery flavor (Chin, Eyres, & Marriott, 2011), while others
such as alkyl- and acetylpyrroles have been linked with negative odors
(Amanpour & Selli, 201 ).
Furan-2-yl-methyl acetate was one of the most abundant compounds
in all evaluated coffee beverages. It is considered a potent odorant in
roasted coffee associated with ethereal-floral and herbal-spicy odor
notes (Caporaso, Whitworth, Cui, & Fisk, 201 ). Furans are mainly
derived from carbohydrate degradation during Amadori rearrangement,
and this degradation is one of the first reactions that occur during coffee
roasting that does not require high temperatures (Toci et al., 2020).
Therefore, it could suggest a trend to higher abundance of furfur-
ylacetate in beverages prepared with the LTLT R s, as observed in our
results.
Regarding to sensory profile, the main roasting effect was significant
for roasted (F) (p = 0.030), woody (F) (p = 0.02 ), malt (F) (p = 0.002),
acidity (p = 0.023), and body (p = 0.014). Irrespective of the BM, coffee
brewed with HTST displayed higher intensity in acidity, woody, malt
flavors, and body (mouthfeel). revious studies have observed differ-
ences in acidity as a function of the roasting degree. Light-roasted degree
coffee has been associated with a significantly higher sour intensity than
dark roasted brewed coffees (Frost, Ristenpart, & Guinard, 2020).
Notably, the same samples (HTST) that showed a higher perceived
acidity also displayed higher TA values and CQAs concentrations.
Although there is a lack of agreement in the relationship between the
titratable and perceived coffee acidity (Cordoba et al., 2020), typically,
perceived acidity is usually primarily attributed to chlorogenic acid and
melanoidins that contain chlorogenic acids (Farah, 2012; Gloess et al.,
2013; Santos, Lopo, Rangel, & Lopes, 201 ). Therefore, it could be
suggested that the higher acidity in coffees brewed with HTST can be
related to fewer acidic molecule degradation and microstructural
changes in the coffee matrix during the roasting process, which favors
the presence of acidic molecules in the final coffee cup. In addition,
coffee samples prepared with HTST showed high body (mouthfeel) in-
tensity, which agrees with the higher TDS values found in these samples.
Our results agree with recent studies that observed an increase in
sourness and thickness (tactile feeling of the liquid in the mouth) with
increase in TDS at different roasting degrees (Frost et al., 2020).
Other flavor notes, such as woody, also showed higher intensity in
the HTST R s. According to the volatiles identified in these samples, the
woody character could be related to a higher presence of some com-
pounds such as phenols and pyrroles in these samples. These compounds
have often been qualified for woody flavor notes (Seninde & Chambers,
2020; Toci & Farah, 2014). In addition, a higher abundance of specific
N. Córdoba et al.

Table 4
Relative abundance (peak area ) of volatile compounds for cold and hot coffee beverages under different roasting conditions.
Brewing method (BM) Cold dripping Cold immersion Hot brewing (French press) Individual factors and
interactions

Roasting profile (RP) HTST LTLT HTST LTLT HTST LTLT RP BM RP:
BM

Compounds RI* (mean ± SD) p-valu

Furans
2-(Methoxymethyl)-furan 1244 0.40 ± 0.23 ± 0.09a 0.1 ± 0.11a 0.45 ± n.da 0.20 ± NS NS NS
0.09a 0.10a 0.09a
Furan-2-carbaldehyde (furfural) 14 12.3 ± 11. 1 ± 13. 4 ± 12.49 ± 12. 2 ± 11. ± NS NS NS
0.4 a 0. 2a 0.39a 0. 0a 0. 9a 1.09a
c
2-(Methylsulfanylmethyl) furan 1494 0.39 ± 0.4 ± 0.19 ± 0.0 0.33 ± 0.03 0. 3 ± 0. 2 ± NS 0.000 0.001
0.0 bc 0.13abc bc
0.04ab 0.0 a
a a b
Furan-2-yl-methyl formate 1501 4.29 ± 3.91 ± 0.4 3.22 ± 0.1 3.10 ± 1. 9 ± 0.1 1.45 ± NS 0.000 0.000
0.25a 0.1 a 0.1 b
1-(Furan-2-yl)-ethanone 151 3.15 ± 3.14 ± 0.15a 3. 1 ± 0.13a 3.5 ± 3.29 ± 0.12a 3.10 ± NS 0.012 NS
0.12a 0.13a 0.15a
a
Furan-2-yl-methyl acetate 1502 1 . 1± 1 .31 ± 1.3 11.04 ± 13.10 ± 11. 1 ± 13.11 ± 0.030 0.000 NS
0. 9a 0.5 b 0.41b 0.40b 0.40b
5-Methylfuran-2-carbaldehyde 15 1 . ± 1 .43 ± 1 . 5± 1 .95 ± 15.41 ± 15. 5 ± NS 0.010 NS
0. 1a 0.54a 0. 4a 0.55a 0.33a 0.55a
Furan-2-yl-methyl propanoate 1 01 0. 2 ± 0. 1 ± 0.04a 0. ± 0.12a 0.53 ± 0. 4 ± 0.05a 0. 4 ± NS NS NS
0.0 a 0.0 a 0.04a
b b a
2-(Furan-2-yl) furan 1 04 0.32 ± 0.2 ± 0.0 0.2 ± 0.11 0.40 ± 1.33 ± 0.0 1.23 ± NS 0.000 0.000
0.0 b 0.0 b 0.0 a
b b a
2-(Furan-2-yl-methyl) furan 1 15 0.34 ± 0.35 ± 0.10 0.30 ± 0.12 0.4 ± 1.34 ± 0.0 1.53 ± NS 0.000 0.000
0.0 b 0.0 b 0.10a
Furan-2-yl-methanol 1 3 10.51 ± 9. ± 0.59a 9. 3 ± 1.50a 11.04 ± 10.2 ± 9. ± NS NS NS
0.41a 1.10a 0. a 0. a
2-(Furan-2-yl-methyl)-5-methylfuran 1 3 n.d c n.d c
n.dc n.d c 0.33 ± 0.03b 0.42 ± NS 0.000 0.000
0.03a
Total 66.73 ± 65.18 ± 60.703 ± 62.40 ± 59.15 ± 59.36 ± NS 0.020 NS
3.20a 4.30a 4.4a 3.44a 2.76a 3.53a

Pyrazines
Methyl-pyrazine 12 5 2. 5 ± 1.95 ± 0.19c 3. ± 0.12a 2. 4 ± 3.04 ± 0.15b 2.3 ± 0.000 0.000 0.000
0.1 b 0.12b 0.14bc
a c
2, -Dimethylpyrazine 133 1. ± 1.49 ± 2.19 ± 0.0 1. ± 1. ± 1.44 ± 0.0 0.000 0.000 0.000
0.0 b 0.0 bc 0.0 b 0.0 bc
a
Ethyl-pyrazine 1344 1. ± 1.40 ± 0.05 1.95 ± 0.0 1.59 ± 1.52 ± 1.29 ± 0.000 0.000 0.000
0.05b cd
0.0 bc 0.04bcd 0.0 d
2,3-Dimethyl-pyrazine 13 0 0.43 ± 0.31 ± 0.03a 0.3 ± 0.03a 0.39 ± 0.3 ± 0.03a 0.29 ± 0.040 NS NS
0.03a 0.03a 0.03a
2-Ethyl- -methylpyrazine 1395 1.23 ± 1.1 ± 1.43 ± 0.12a 1.1 ± 1.00 ± 0.04b 0.94 ± NS 0.002 NS
0.05ab 0.04ab 0.0 ab 0.0 b
a b
2-Ethyl-5-methylpyrazine 1402 1.0 ± 1.01 ± 1.1 ± 0.09 1.02 ± 0. 5 ± 0.03 0. 4 ± NS 0.001 NS
0.03ab 0.012ab 0.0 ab 0.05b
2-Ethyl-3-methylpyrazine 1415 0. 9 ± 0. 1 ± 0.91 ± 0.05a 0. 2 ± 0.59 ± 0.03c 0.5 ± 0.04c 0.015 0.000 NS
0.03ab 0.03bc 0.04bc
3-Ethyl-2,5-dimethyl-pyrazine 1442 0.51 ± 0.54 ± 0.05a 0.4 ± 0.49 ± 0.29 ± 0.04b 0.35 ± NS 0.004 NS
0.05ab 0.04ab 0.04ab 0.0 ab
Total 10.31 ± 8.56 ± 0.46 12.24 ± 9.99 ± 9.30 ± 8.11 ± 0.000 0.000 NS
0.49b cd
0.58a 0.49bc 0.41bcd 0.54d

Pyrroles
a
1-Methylpyrrole-2-carbaldehyde 1 3 1.21 ± 1.44 ± 0.0 1.0 ± 0.11b 1.24 ± 0.91 ± 0.04b 1.22 ± 0.002 0.011 NS
0.0 ab 0.09ab 0.04ab
c
1-(Furan-2-yl-methyl) pyrrole 1 3 0. ± 0. 5 ± 0.54 ± 0.33 ± 0.0 1.20 ± 0.09a 1.25 ± NS 0.000 0.000
0.12b 0.13bc 0.05bc 0.05a
1-(1H-pyrrol-2-yl) ethanone 19 2 0.34 ± 0.30 ± 0.24 ± 0.02b 0.2 ± 0.2 ± 0.2 ± NS 0.010 NS
0.02a 0.02ab 0.01ab 0.02ab 0.02ab
1H-pyrrole-2-carbaldehyde 203 0.4 ± 0.49 ± 0.03a 0.33 ± 0.02c 0.42 ± 0.3 ± 0.40 ± 0.025 0.005 0.010
0.04ab 0.03abc 0.02bc 0.03abc
Total 2.78 ± 3.0 ± 0.23a 2.18 ± 2.25 ± 2.74 ± 3.14 ± NS 0.000 NS
0.25ab 0.20b 0.24b 0.17ab 0.15a

Phenols
2-Methoxyphenol 1 0 0.3 ± 0.33 ± 0.03a 0.20 ± 0.0 a
0.2 ± 0.3 ± 0.04a 0.3 ± NS 0.052 NS
0.03a 0.0 a 0.04a
henol 2011 n.da n.da n.da n.da 0.12 ± 0.04a n.da 0.01 NS NS
b b
4-Ethenyl-2-methoxyphenol (4- 220 0. 5 ± 0.4 ± 0.0 0.4 ± 0.0 0.42 ± 1.04 ± 0.0 a 0. 2 ± 0.003 0.000 0.000
vinylguaiacol) 0.05a 0.0 b 0.0 a
Total 1.21 ± 0.81 ± 0.81 ± 0.70 ± 1.53 ± 1.19 ± 0.005 0.000 NS
0.09ab 0.10bc 0.18bc 0.14c 0.13a 0.11ab

Furanones
a a
2-Methyloxolan-3-one 12 3 0. 5 ± 0.0 0. 5 ± 0.0 0.001 0.039 NS
(continued on next page)
N. Córdoba et al.

Table 4 (continued )
Brewing method (BM) Cold dripping Cold immersion Hot brewing (French press) Individual factors and
interactions

Roasting profile (RP) HTST LTLT HTST LTLT HTST LTLT RP BM RP:
BM

Compounds RI* (mean ± SD) p-valu

0. ± 0.95 ± 1.21 ± 0.9 ±

0.0 a 0.0 ab 0.10b 0.0 ab
5-Methyl-3H-furan-2-one 144 0.29 ± 0.2 ± 0.05a 0.2 ± 0.04a 0.32 ± 0.25 ± 0.0 a
0.23 ± NS NS NS
0.05a 0.05a 0.09a
Total 0.95 ± 1.20 ± 1.11 ± 1.53 ± 1.10 ± 1.19 ± 0.008 NS NS
0.11b 0.12ab 0.11ab 0.15a 0.14ab 0.16ab

Ketones
entane-2,3-dione 10 0 0. 3 ± 1.14 ± 0.24a 0. 9 ± 0.21a 1.23 ± 0.45 ± 0.21a 0.31 ± NS 0.021 NS
0.19a 0.2 a 0.1 a
2-Oxopropyl acetate 14 1 0. ± 0. 1 ± 0.03b 0. ± 0.04a 0. ± 0. 5 ± 0. 2 ± 0.005 0.01 0.000
0.04ab 0.0 ab 0.04ab 0.0 b
Total 1.40 ± 1.75 ± 1.75 ± 2.01 ± 1.21 ± 0.93 ± NS 0.010 NS
0.23ab 0.26ab 0.26ab 0.34a 0.24ab 0.23b

Aldehydes
2-methylbutanal <1000 2.19 ± 3.12 ± 0.09a 2.29 ± 1. 3 3. ± 1. 0 ± 0.9 a
1.9 ± NS NS NS
1.32a a
0.91a 0.4 a
3-methylbutanal <1000 nda nda
nd a
nda 0.22 ± 0.01 b
0.41 ± 0.05c NS 0.001 NS
Total 2.19 ± 3.12 ± 2.29 ± 3.66 ± 1.82 ± 2.38 ± NS NS NS
1.32a 0.09a 1.83a 0.91a 0.57a 1.10a

Acids
Acetic acid 145 0.19 ± n.db 0.2 ± 0.04a 0.32 ± n.db n.db NS 0.000 0.002
0.0 a 0.05a

Pyridines
yridine 1190 0.4 ± 1.45 ± 0. 3a 1.4 ± 0. a
1. ± 0. ± 0. 3a 1. 0 ± NS NS NS
0. 3a 0. 0a 0. 3a

* Average experimental retention index. Values are shown as means ± standard deviation (n = 3). Different letters on the same raw means that the data are significantly
different (p < 0.05). NS, not significant effects (p > 0.05). R Roasting rofile, BM Brewing Method, R BM Roasting profile Brewing method interaction, CD Cold
dripping, CI Cold immersion, HB Hot brewing, HTST (High-temperature short time), LTLT (Low-Temperature Long Time). n.d = not detected.

pyrazines (e.g., ethylpyrazine and 2-ethyl- -methylpyrazine) have been
related to woody/papery flavor notes (Maeztu et al., 2001) found in
HTST, and could be associated with the higher intensity of perceived
woody notes. On the other hand, all samples prepared with LTLT showed
higher intensity in roasted flavor. These results agree with previous
findings showing that the most intense roasted flavor is related to the
dark roast level, and the roasting times in this process are close to those
used in the present investigation (15 min) (Frost et al., 2020). Likewise,
cold brew coffees have found higher roasted intensities in flavor when
dark roasted levels have been used (Seninde et al., 2020).
3.2. Effect of BM
The main effect of the BM was significant (p < 0.05) for all physi-
cochemical characteristics evaluated (TDS, EY, pH, and TA). Cold cof-
fees brewed by CD exhibits the highest values of TDS and EY followed by
CI and HB (Table 2-I). A similar trend is present in the non-volatile
concentration where, regardless of the R , CD presents a higher con-
centration (p < 0.05) of caffeine, trigonelline, and 4-and 5-CQA
(Table 2-II-B). revious studies on these cold BMs have observed a
similar trend in caffeine and CQA concentrations (Angeloni, Guerrini,
Masella, Bellumori, et al., 2019; Angeloni, Guerrini, Masella, Innocenti,
et al., 2019). HB displayed the highest TA values for both R s. Similar
results were reported by Rao & Fuller (201 ), who explained that the
differences in TA between hot and cold brew coffees are related to the
effect of water temperature on the extraction and transport of acidic
molecules from the coffee matrix into the water phase.
Extraction efficiency can be defined as the ratio of the mass of the
coffee material that passes into the cup and the total ground coffee used
(Clarke & Vitzthum, 2001). The results show higher extraction effi-
ciency (mg/g coffee ground) for CD, followed by CI and HB (Table 2-II-
B). revious studies comparing several HB methods and CD also found
that the hot coffees brewed by French ress displayed less efficiency in
the extraction of caffeine and CQAs (Angeloni, Guerrini, Masella, Bel-
lumori, et al., 2019; Angeloni, Guerrini, Masella, Innocenti, et al., 2019).
Despite the low non-volatile concentration in HB, this BM displays
the highest extraction rate (Fig. 2). The extraction rate for each non-
volatile compound was calculated considering the relation between
the extraction efficiency and the extraction time used in each BM. These
results were expected because French ress is considered a full immer-
sion technique where the ground coffee and water are well mixed (Frost,
Ristenpart, & Guinard, 2019). This fact, together with higher tempera-
tures (90 ± 3 ◦ C) used in HB, help facilitate more soluble and volatile
compounds to be present in the drink in less time (5 min), compared to
cold methods that require longer times ( –14 h) to compensate for the
low temperature (19 ± 2 ◦ C). Among cold BMs, the non-volatile
extraction rate showed significant differences (p < 0.05) between the
two methods evaluated. In general, CD exhibits higher extraction rates
than CI for all compounds (Fig. 2). The highest concentration and
extraction rate observed in CD are related to the physical characteristics
of each system, which determine the extraction dynamics and mass
transfer during the process. The CD system allows continuous water
renewal, while in CI, the grinding coffee remains static and directly
immersed in the aqueous solution. CD is more efficient when extracting
different molecules compared to a static system because the concen-
tration gradient drives the matter transfer from the solid to the liquid
phase (Angeloni, Guerrini, Masella, Innocenti, et al., 2019).
Although the long durations and configurations of the system in CD
can increase efficiency and extraction rate, it is important to note that
long contact times can lead to under or over-extraction of other com-
pounds that affect the coffee flavor. Some studies have quantified higher
chlorogenic acid lactones (CGLs) in cold drips than immersion coffee
brews (Angeloni, Guerrini, Masella, Innocenti, et al., 2019). Likewise, a
higher concentration of CGLs were observed in CD than in French ress
N. Córdoba et al.
Fig. 2. Extraction rate for non-volatile compounds in cold and hot brew coffees. Statistical significance was examined using ruskal-Wallis test, NS not significant *
significant at level α = 0.05. 5-CQA 5- Caffeoylquinic acid, 4-CQA 4- caffeoylquinic acid, HTST (High - Temperature Short Time), LTLT (Low - Temperature Long
Time). Brewing methods CD Cold dripping, CI Cold Immersion, HB Hot brewing. Extraction rate (mg/g coffee ground*h), regarding the amount of ground coffee
used by the time employed in each brewing method.
(Angeloni, Guerrini, Masella, Innocenti, et al., 2019). CGLs have been
identified as the main contributors to bitterness in coffee (Frank,
Zehentbauer, & Hofmann, 200 ). Therefore, their higher abundance
could partly explain the higher bitterness associated with the brews
created by CD.
Likewise, the concentration of the non-volatile compounds per 100
mL of brew showed that cold drip samples had the highest caffeine
concentration average of 13 . mg / 100 mL. These values are close to
the previously reported caffeine concentration at 142.5 mg / 120 mL
for the same cold method (Angeloni, Guerrini, Masella, Innocenti, et al.,
2019). However, some commercial cold brew studies have also reported
lower concentrations at 20 mg / 12 fl. Oz (Lane, almer, Christie,
Ehlting, & Le, 201 ). The lowest caffeine content was observed in HB
( 0. 4 mg / 100 mL). revious studies have observed this same trend
and they have reported a caffeine content in coffee infusions brewed by
French ress at 2.1 mg / 120 mL (Angeloni et al., 2019).
Considering the volatile compounds, the BM was significant for 24 of
the 35 volatile compounds identified. Overall, the highest numbers of
volatile compounds (in order of abundance) were furans and pyrazines,
which together accounted for more than 0 of the compounds found in
all assessed coffee drinks. The data showed that the total peak area ( )
of furans was affected by the BM (p = 0.020). A higher total abundance
of these compounds was found in cold brew coffees, mainly in those
brewed by CI, which were different (p < 0.05) than in HB. In general, the
most abundant specific furans in all coffee beverages were 5-methyl-
furan-2-carbaldehyde (5-methyfurfural), furan-2-yl-methyl acetate,
furan-2-yl-methanol (2-furanmethanol) and furan-2-carbaldehyde
(furfural). The abundance of furan-2-yl-methyl acetate is higher in CD
(1 ), and the value exhibits significant differences (p < 0.05) with CI
(12.1 ) and HB (12.4 ) (Table 4). Based on the odor activity value,
furan-2-yl-methyl acetate (fruity, ester-like, roast, and sweet) has been
suggested as one of the most important furans in terms of its strong
impact on aroma related to sweet, fruity bread-like, roast, and caramel
odor notes in hot coffee beverages (Amanpour & Selli, 201 ).
Other furans, such as 2-(furan-2-yl)furan, (2-(furan-2-yl-methyl)
furan), (2-(furan-2-yl-methyl)-5-methylfuran and 2-(methyl-
sulfanylmethyl)furan are more abundant (p < 0.05) in HB than in cold
brew coffees (Table 4). These compounds also showed a significant ef-
fect between the interaction of R and BM. Furans and its derivative
compounds are generated upon roasting from thermal degradation, and
their concentration in the cup depends on the BM, among other factors
(La era et al., 2009; Rahn & Yeretzian, 2019). 2-(furan-2-yl-methyl)
furan and 2-(furan-2-yl)furan have been referenced to possess green and
medicinal flavor notes (Flament, 2002) and 2-(methylsulfanylmethyl)
furan have been associated with sulfur, garlic, smoke, and roasted odor
notes (Caporaso, Genovese, Canela, Civitella, & Sacchi, 2014; Flament,
2002).
The effect of BM was significant for total pyrazines (p = 0.000). CI
showed a higher abundance in the total peak area ( ) of pyrazines and
in specific compounds such as methyl-pyrazine, ethylpyrazine, and 2, -
dimethyl pyrazine, which were superior to the values observed for HB
and CD. For these specific compounds, the interaction between R and
BM was also significant (p < 0.05). This interaction can be related to the
roasting process, wherein many of these compounds are generated and
the extraction conditions dictate their concentrations in the brew. In
general, high temperatures favor the extraction of several VOCs. How-
ever, its extraction does not only depend on the compound’s volatility,
but also on other chemical properties, such as solubility and polarity,
which modulate the final composition of the coffee brew (Cordoba et al.,
2020).
Total ketones were significantly (p = 0.010) affected by the BM. In
general, a higher total abundance was observed in cold brew coffees
than in hot brew coffees (p < 0.05). 2,3-pentanedione and 2-oxopropyl
acetate (1-(acetyloxy)-2-propanone) were more abundant in CI. etones
have been considered as important molecules in determining coffee
aromas with fruity, buttery, and dairy notes (Caporaso, Whitworth,
Grebby, & Fisk, 201 ), and their extraction concentrations can vary
depending on the coffee BM. For instance, López-Galilea, Fournier, Cid,
N. Córdoba et al.
& Guichard (200 ) reported that ketones were more abundant in filtered
than espresso coffee beverages. Likewise, 1-(acetyloxy)-2-propanone
presence in both hot and cold coffee beverages could be related to its
high solubility in water (1.52E + 05 mg / mL) (Bressanello et al., 201 ).
Although a trend for the formation of specific ketones, with regards to
the roasting conditions, has not been observed (Gloess et al., 2014),
some ketones can be affected by the roasting conditions (Baggenstoss
et al., 200 ) which can explain the significant (p = 0.000) interaction
between R BM observed in 1-(acetyloxy)-2-propanone.
Total pyrroles were affected (p = 0.000) by the BM; CI showed a
higher abundance (2.21 ), followed by CD (2. ), and HB (2.94 ).
Recent studies have also reported a comparable abundance of pyrroles in
cold brews prepared by CI (3.12–3.14 ) and CD (3.11–3.20 ) ( ang,
Lee, Davaatseren, & Chung, 2020). Although pyrroles are produced
upon the roasting process, after being roasted, some of these compounds
continue to be affected by the brewing conditions, their intrinsic insta-
bility, and interactions with coffee matrix components (Charles-Ber-
nard, raehenbuehl, Rytz, & Roberts, 2005). In this sense, Charles-
Bernard et al. (2005) have observed that some compounds present in the
coffee brew (e.g., melanoidins) induce retention for di-ketones and
pyrrole-derivatives. These facts can be explained by the significant
interaction R BM observed in 1-(furan-2-yl-methyl) pyrrole (p = 0.000)
and 1H-pyrrole-2-carbaldehyde (p = 0.010).
Moreover, the BM affected the extraction of total phenols (p =
0.000); HB showed higher abundance of phenols in than cold brew
coffees. Among phenolic compounds, the BM was significant (p = 0.000)
for 4-ethenyl-2-methoxyphenol (4-vinyl guaiacol), which showed a
higher abundance in HB (0.93 ), followed by CD (0. ), and CI
(0.45 ). Likewise, the interaction R BM was significant (p = 0.000) for
this compound, which was consistent given that the formation of 4-vinyl
guaiacol is highly dependent on the roasting process (Baggenstoss et al.,
200 ).
Among other VOC compounds, the BM had an effect on aldehydes
including 3-methylbutanal (p = 0.001), which was only detected in HB.
This compound has been associated with a high impact on the flavor of
coffee, related to malty and cocoa notes ( oisson, Blank, Dunkel, &
Hofmann, 201 ). Likewise, the BM had a significant impact on acetic
acid (p = 0.000). This compound is detected mostly in cold brew coffees
but is not observed in HB (Table 4). Recent studies on cold brew using
Fig. 3. Sensory profiles for cold brews (dripping and immersion) and hot brews brewed with coffees at different roasting profiles. Mean intensities by significant
attributes (p < 0.05) for brewing method (*), roasting profile (**) and their interaction (***) for descriptive attributes are shown. CD Cold dripping, CI Cold
Immersion, HB Hot brewing, HTST (High - Temperature Short Time), LTLT (Low - Temperature Long Time). F indicate attributes descriptive of flavor, AR; aroma,
and M mouthfeel. For p-values of individual factors and their interactions for all coffee attributes evaluated see Supplementary Table S1.
dripping and immersion methods have reported an average of 0.2
acetic acid content in these coffee beverages (Han, Boo, & Chung, 2020),
and this value is close to those found in the present work (0.19–0.32 ).
Acetic acid was also affected by the interaction between R and BM. In
this regard, previous studies have observed that this compound is highly
affected by the roasting process and is most abundant at the medium
roast level (Yeretzian, ordan, Badoud, & Lindinger, 2002).
Regarding the effect of the BM on the sensory profile, the results
showed that this variable had a significant effect on nutty (F) (p =
0.01 ), floral (F) (p = 0.009), and sweetness (p = 0.035). In general, CI
exhibited a higher intensity in these three attributes. Sweetness intensity
was comparable with HB, while lower intensities for these attributes
were observed in CD. In general, cold brew samples obtained by CI
showed a similar profile to HB, mostly in some attributes such as
sweetness, nutty, acidity, floral and malt flavor, and vanilla aroma
(Fig. 3). revious studies in cold brew coffee have shown that the
extraction method influences the intensity of sweet flavor and related
attributes (caramel, malty, fruity, and floral flavor) (Angeloni et al.,
2019; Cordoba, ataquiva, Osorio, Moreno, & Ruiz, 2019; Han, Boo, &
Chung, 2020). Likewise, using a hedonic scale and an overall preference
ranking test, Han et al. (2020) observed that cold immersion was
characterized mainly by the sweetness and cold dripping by a higher
bitter intensity. These dissimilarities could be related to the caffeine
content, which is higher in cold dripping than immersion (Angeloni,
Guerrini, Masella, Innocenti, et al., 2019). Similar to previous findings,
our results showed that CI and HB showed a lower content of non-
volatile compounds and TDS, which could explain the higher sweet-
ness perceived in the resulting beverages. In this sense, recent studies
have found similar trends in which sweetness exhibited an inverse cor-
relation with TDS irrespective of the degree of roasting (Frost et al.,
2020).
Other sensory attributes were also affected by the interaction of R
BM; among them, vanilla (AR/F) (p = 0.01 / p = 0.003) showed higher
intensity in HB-LTLT, and this balance (p = 0.040) was higher in HB-
HTST. On the other hand, caramel (F) (p = 0.020) and aroma (p =
0.025) increased in CI-LTLT, while malt (F) intensity (p = 0.005) was
higher in CI when HTST profile was used. In this sense, recent studies in
cold brew sensory profiles have suggested a key role in the interactions
between several factors (e.g., coffee bean species, roasting degree, coffee
N. Córdoba et al.

to water ratio, and BM) on the cold brew sensory characteristics
(Seninde et al., 2020).
3.3. Principal components analysis (PCA)
CA was performed to examine the differences or similarities be-
tween the coffee samples (Fig. 4). The first component represented the
temperature of the brew, with 31.44 of the variance obtaining positive
values in hot brewed samples. The second component, with a variance
explanation of 21. , separated across R s. The impact of the R was
most evident in beverages prepared with hot water and two clusters, one
for each R , was observed. However, such separation was not clearly
defined for cold brews, with the exception of LTLT, which was separated
when CD was used in brewing. As shown in Fig. 4, hot coffee infusions
were distributed across the positive side, while cold infusions were
located on the negative side, indicating that the dominant effect was
primarily influenced by the brewing temperature. Hot coffees brewed by
French ress depicted the highest relation with some volatile com-
pounds such as 2-(furan-2-yl-methyl)furan, 2-(furan-2-yl)furan, 2-
(furan-2-yl-methyl)-5-methylfuran, 2-(methylsulfanylmethyl)furan, 4-
ethenyl-2-methoxyphenol, 1-(furan-2-yl-methyl)pyrrol and 3-methylbu-
tanal, as well as with the total titratable acidity.
Cold drip coffees were mostly associated with high concentrations of
caffeine, trigonelline, and total caffeoylquinic acids. They displayed a
positive correlation with TDS and a higher bitterness and roasted flavor,
mainly for those prepared with the LTLT R . In contrast, coffee bever-
ages with the highest intensity in sweetness and sweet-associated attri-
butes (CI and HB) showed a negative correlation with the concentration
of TDS, caffeine, trigonelline, and CQAs. Recent studies by Batali et al.,
(2020), have suggested that noticeable sweetness in coffee is a conse-
quence of masking effects and / or the presence of sweet-associated
aromas and flavor. For instance, perception of sweetness could
increase in the presence of sweet-associated aromas; oppositely, some
degree of masking could be given due to a dominate related to sour‑ and
bitter-tasting compounds that could be masking other more delicate
flavors (Batali, Frost, Lebrilla, Ristenpart, & Guinard, 2020). These facts
could be related to the trends found in our results, where beverages with
the highest bitter flavor (CD) exhibited a low sweetness intensity.
Cold brew coffees prepared by immersion were mainly defined by
the presence of volatile compounds such as ketones, furans, furanones,
and pyrazines, which are related to sensory attributes found in the same
quadrant, such as nutty, caramel, and malt.
4. Conclusions
This study indicates differences between coffee brews, mainly by the
brewing method. Brewing method using hot water (90 ± 3 ◦ C) allowed a
more distinct discrimination of coffee beverages brewed with HTST and
LTLT R s. Hot coffee brews were separated from cold brew mainly by a
higher TA and abundance of some compounds such as 2-(furan-2-yl-
methyl)furan, 2-(furan-2-yl)furan, 2-(furan-2-yl-methyl)-5-methyl-
furan, 2-(methylsulfanylmethyl)furan, 4-ethenyl-2-methoxyphenol, 1-
(furan-2-yl-methyl)pyrrol and 3-methylbutanal, as evidenced in the hot
coffee samples. Technical differences associated with the BMs generated
quantitative differences in TA, TDS, caffeine, trigonelline, CQAs, and
volatile compounds, which were reflected in coffee brews with a
different sensory profile. Notably, the cold dripping method generated
beverages with higher TA, TDS, caffeine, trigonelline, and CQAs, and
displayed higher bitterness and roasted flavors. In contrast, the cold
immersion and hot brewing (French ress) coffee beverages showed
remarkable intensity in sweetness attributes, which showed a negative
correlation with the concentration of caffeine, trigonelline, CQAs, and
TDS.
It is worth pointing out that the chemical composition of coffee can

Fig. 4. rincipal component analysis ( CA) of chemical and sensory characteristics of cold and hot brew coffees. HT HTST (High - Temperature Short Time), LT
LTLT (Low - Temperature Long Time). Brewing methods CD Cold dripping, CI Cold Immersion, HB Hot brewing. TDS Total dissolved solids, TA Titratable acidity,
T.CQAs Total Caffeoylquinic acids. For volatile compounds, the figure includes short chemical names. I AC names that were not included are listed in parentheses
in italic. 2- (Methylthio)methyl -furan (2-(methylsulfanylmethyl)furan) 1-Furfurylpyrrole (1-(furan-2-yl-methyl)pyrrole) 2-(2-Furanylmethyl)-5-methyl-furan (2-
(furan-2-yl-methyl)-5-methylfuran); 2,2′ -Methylenebis-furan (2-(furan-2-yl-methyl)furan); 2,2′ -Bifuran (2-(furan-2-yl)furan); 2-Methoxy-4-vinylphenol (4-ethenyl-2-
methoxyphenol); Dihydro-2-methyl-3(2H)-furanone (2-methyloxolan-3-one); 2-Furanmethanol (furan-2-yl-methanol); 2,3- entanedione (pentane-2,3-dione); 5-Methyl-2
(3H)-furanone (5-methyl-3H-furan-2-one); 2-Furfurylformate (furan-2-yl-methyl formate); 1-Methyl-1H-pyrrole-2-carboxaldehyde (1-methylpyrrole-2-carbaldehyde);
Furfurylacetate (furan-2-yl-methyl acetate); 5-Methylfurfural (5-methylfuran-2-carbaldehyde).
N. Córdoba et al.
change depending on its origin, variety, environment, and management.
However, the results found in this study allow us to determine how the
roasting conditions, water temperature, and technical BM characteris-
tics influence observable differences in the extraction of certain chem-
ical compounds that affect the sensory profile of the resulting beverages.
These results could provide new insights for future work related to cold
extraction methods and their operative variables to elucidate how the
extraction rates of chemical compounds could produce cold brew coffees
with different flavor profiles.
CRediT authorship contribution statement
Nancy Córdoba: Investigation, Methodology, Formal analysis,
Visualization, Writing - original draft. Fabian L. Moreno: Formal
analysis, Writing - review & editing, Supervision. Coralia Osorio: Su-
pervision, Validation, Writing - review & editing. Sebastián Velásquez:
Formal analysis, Data curation, Visualization. olanda Ruiz: Concep-
tualization, Resources, Writing - review & editing, Supervision, ro ect
administration, Funding acquisition.
Declaration of Competing Interest
The authors declare that there is no conflict of interest.
Ac nowledgments
The authors wish to thank Dra. Tatiana Cuadrado for her support
during S ME-GC/MS analysis. Besides, Sara orras and ulio Villaneda
of Café 1 /Banexport for their support in the coffee roasting process.
Thanks to Norbert Niederhauser, Cropster CEO, who generously pro-
vided free access to Cropster roasting intelligence software. Further-
more, we are grateful to the sensory panel, trained assessors of
Colombian specialty coffee companies Café y rocesos (Hernando
Tapasco), Cafecultor/Inconexus ( uan Espinel), Devoción (Salomón
Winograd, Daniel Romero), Café 1 /Banexport ( ulio Villaneda), Luis
Felipe Tru illo, niversidad de La Sabana (Annamaria Filomena, M.Sc;
Dr. Leonardo Moreno). We are grateful to Manuel Osorio, M.Sc., and
Laura ataquiva, M.Sc. Finally, to all the volunteer students and Engi-
neering faculty staff ( niversidad de La Sabana) that supported the lo-
gistics for the sensory analysis sessions. Last but not least, to ARCAFE
Linares and Fidencio Chamorro for providing the coffee.
Funding
This work was supported by niversidad de La Sabana, the Coffee-
lands rogram of Catholic Relief Services (CRS) grant number ING-1 0-
201 and MINCIENCIAS (Colombia) doctoral scholarship for the author
N.Cordoba grant number 2 -2015 .
Appendix A. Supplementary material
Supplementary data to this article can be found online at https //doi.
org/10.101 / .foodres.2021.110141.
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