Food Chemistry 381 (2022) 132215

Contents lists available at ScienceDirect

Food Chemistry
journal homepage: www.elsevier.com/locate/foodchem

Impact of using cocoa bean shell powder as a substitute for wheat flour on
some of chocolate cake properties
Fabíola Nogueira Soares Souza a, Suellen Rocha Vieira b,
Marina Leopoldina Lamounier Campidelli c, Renata Abadia Reis Rocha c,
Leonardo Milani Avelar Rodrigues d, Pedro Henrique Santos e, João de Deus Souza Carneiro c,
Iasnaia Maria de Carvalho Tavares a, Cristiane Patrícia de Oliveira a, *
a
Department of Exact Sciences and Natural, State University of Southwest Bahia, 45700-000 Itapetinga, Brazil
b
Department of Chemical Engineering, Federal University of Bahia, 40210-630 Salvador, Brazil
c
Department of Food Science, Federal University of Lavras, Zip: 37200-000, Lavras, MG, Brazil
d
Department of Exact Sciences and Natural, University Center of the Americas, 01304-001 São Paulo, Brazil
e
Department of Chemical Engineering and Food Engineering, Federal University of Santa Catarina, 88040-900, Florianópolis, Brazil

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

Keywords: The cocoa bean shell is a residue rich in bioactive compounds and its use as an ingredient in the food industry has
Agroindustrial waste been studied. This work had the objective of proposing the elaboration of chocolate cake with substitution of
Antioxidant activity wheat flour by cocoa bean shell powder (CSp). Five formulations with different percentages of CSp were used:
Bioactive compounds
25%, 50%, 75%, 100% and 0% (control). The cakes were evaluated by technological characteristics (volume,
Sensory analysis
Bakery products
texture profile, firmness and colour), antioxidant profile (DPPH, β-carotene/linoleic acid system, phenolic
Theobroma cacao compounds, anthocyanins and tannins) and sensory tests (TDS and acceptance). The technological characteristics
and antioxidant activity of the cakes were influenced by the different concentrations of CSp compared to the
control sample. The cakes containing up to 75% CSp presented satisfactory sensory acceptance. Therefore, CSp
has been revealed to be a prominent alternative substitute ingredient to be used promisingly in the food industry.

1. Introduction production of biofertilizers, biogas, briquettes, films and microbial en­

The food industry generates, throughout its production and pro­
cessing chain, a large amount of agro-industrial waste (Lessa et al.,
2018). Specifically, in the fruit processing industries, waste makes up
about 65 % to 70 % of the total fruit mass, with some variation,
depending on the species of the fruit (Sousa et al., 2011). In recent years,
several researchers have studied the use of this waste, such as fruit peels
and seeds, for the production of food or ingredients such as flour (de
Barros et al., 2020; Resende, Franca, & Oliveira, 2019), avoiding the
inappropriate disposal of these usually inedible parts.
In the cocoa (Theobroma cacao L.) production chain, for chocolate
production, a large amount of vegetable waste is generated. Three kinds
of by-products are generated, the cocoa pod husks, cocoa bean shells and
cocoa mucilage (Lessa et al., 2018; Martínez et al., 2012; Panak Balentić
et al., 2018). To address this problem, new technologies have been
stimulated, aiming to reduce these residues, using them in the
zymes to accelerate the production of biofuel and, in this way, taking full
advantage of the cocoa fruit (Ferrão-Gonzales, Vital, Lima, & Rodrigues,
2013; Lessa et al., 2021; Sales de Menezes et al., 2021). In general, the
residues from the cocoa processing industries are destined for non-food
purposes (Lessa et al., 2018).
The cocoa bean shell is the outer part of the cocoa bean removed
after roasting, which represents 10 %–17 % of the cocoa seed, however,
this percentage can vary significantly, as in other vegetables, depending
on climatic factors, cocoa variety, processing conditions, among others
(Rojo-Poveda et al., 2019). This residue is a rich source of carbohydrates
(178.0 ± 0.9 g/kg) and proteins (150 ± 2 g/kg), presenting a low lipid
content (20.2 ± 0.3 g/kg) (Martínez et al., 2012). In addition, cocoa
pods have a high nutritional value, containing a variety of bio­
composites, including alkaloids such as theobromine and methylxan­
thine, dietary fibre and phenolic compounds (Okiyama, Navarro, &
Rodrigues, 2017). Lessa et al. (2018), when analysing the compounds

* Corresponding author.
E-mail address: cristianepatricia@uesb.edu.br (C. Patrícia de Oliveira).

https://doi.org/10.1016/j.foodchem.2022.132215
Received 1 April 2021; Received in revised form 23 December 2021; Accepted 19 January 2022
Available online 22 January 2022
0308-8146/© 2022 Elsevier Ltd. All rights reserved.
F. Nogueira Soares Souza et al.
present in the cocoa shell in the natural state and after fermentation,
found high values of antioxidant and phenolic capacity (2120 mg of
gallic acid per 100 g of cocoa bean shell), as well as the presence of
carotenoids (0.8 mg of β-carotene per 100 g of cocoa bean shell), an­
thocyanins (0.4 µg of quercetin per 100 g of cocoa bean shell) and fla­
vonols (1.5 µg of quercetin per 100 g of cocoa bean shell). Therefore, the
cocoa hull is considered to be rich in bioactive compounds. In this way,
the development of cocoa bean shell products intended for human
consumption may be a viable alternative to add value to this whole
process.
Some studies and patents have been developed to give an adequate
end to this product in several areas (Jahurul et al., 2013; Mancini,
Papirio, Lens, & Esposito, 2016). In food science and technology, cocoa
bean shell has been applied as an intermediate ingredient for functional
foods (Martínez et al., 2012), such as cereal bars (Barros et al., 2021),
where the sample was powdered before addition to the product, and
chocolate (Barišić et al., 2020) because it is a source of fibre and
bioactive compounds with antioxidant properties.
Specifically, in bakery products, use of cocoa bean shell has been
widespread and appreciated because, in addition to enriching these
products, this raw material, after being crushed and transformed into
flour, may provide products with sensory characteristics close to or even
the same as those of the originals by simply replacing wheat flour with
cocoa bean shell flour. The literature presents some studies that report
the use of cocoa bean shell as raw material, in powder form, in biscuits
(de Barros et al., 2019), in the form of alkalized dietary fibre in biscuits
(Handojo, Triharyogi, and Indarto (2019)) and in the form of dietary
fibre in bread making (Collar, Rosell, & Muguerza, 2009). The
replacement of wheat flour with cocoa bean shell flour in cake
manufacturing is an application that needs to be studied. However, ac­
cording to Okiyama et al. (2017), cocoa bean shell may be applied in the
food industry as an ingredient of outstanding versatility, promoting the
addition of the desired cocoa flavour and the incorporation of bioactive
compounds and fibres in several products, including bakery products.
Therefore, this research aimed to: (i) evaluate cocoa bean shell
powder (CSp) in terms of physical and chemical characteristics; (ii) use
CSp to make a cake, followed by evaluation of its physical, chemical and
sensory characteristics.
2. Material and methods
2.1. Raw material and sample preparation
The cocoa bean shells were kindly provided by chocolate producers
from Ilhéus – Bahia, Brazil. The raw material was then inserted into
polyethylene bags and stored at room temperature until the following
experiments. Samples from three different chocolate productions were
used, thus configuring three repetitions, disregarding the cocoa variety
and its respective production period.
The CSp was obtained by ball-milling (Marconi MA350, Piracicaba –
SP) and sieving. Finally, the samples were stored in vacuum packages at
room temperature until analysis.
The extract solution (ES) used to determine antioxidant activity by
the DPPH method, antioxidant activity by the beta-carotene/linolenic
acid systems, anthocyanin content and total phenolic content by
Folin–Ciocalteu reagent was obtained by cold extraction, by shaking 40
g of cocoa bean shell in natura with 80 % hydroethanolic solution for 1
h, in a 1:7 shell : solvent ratio (Lessa et al., 2018). The extract was
conditioned in amber bottles under refrigeration until carrying out the
analyses.
2.2. Raw material analysis
2.2.1. Proximate analysis and total acidity
Determination of moisture, carbohydrate, lipid, protein and ash
content, along with total acidity, was carried out according to AOAC
2
Food Chemistry 381 (2022) 132215
(2010).
2.2.2. Specific composition
2.2.2.1. Analysis of total soluble sugars. The soluble sugar content was
determined by the anthrone method described by Hodge and Hodfreiter
(1962). First, 1 g of the sample and 80 mL of 80 % ethanol were mixed
and inserted into a boiling water bath for 1 h. Afterward, the sample was
allowed to stand for 16 h and filtered on WhatmanTM filter paper with
14 µm porosity. The filtrate was placed in a 250 mL conical flask, washed
with 25 mL of 95 % ethanol and heated on a hot plate until complete
evaporation. Subsequently, the extract was poured into a 100 mL beaker
and the volume was completed with distilled water. Next, 1 mL of the
diluted extract was mixed with 2 mL of the anthrone reagent in a beaker,
which was placed into a boiling water bath for 8 min. Finally, the
samples were cooled in an ice bath and the reading was done at 620 nm
in a spectrophotometer.
2.2.2.2. Analysis of mineral composition. The mineral composition of the
CSp samples was determined according to Malavolta, Vitti, and Oliveira
(1997). First, the samples were submitted to nitroperchloric digestion
(NPD). The NPD extracts were then used for analysis of mineral
composition in which their average levels of P, K, Ca, Mg, S, B, Cu, Mn,
Zn and Fe were determined. The K content was analysed by flame
photometry, the P content by colorimetry using the molybdovanadate
method, the S content by turbidimetry and the Ca, Mg, B, Cu, Zn, Mn and
Fe content by atomic absorption spectrometry.
2.2.2.3. Fatty acid profile. Fatty acids were extracted using the Soxhlet
method (AOAC, 2010). Subsequently, fatty acid methyl esters (FAMEs)
were prepared according to the methodology proposed by AOAC (2010).
The FAMEs were analysed by a Thermo Finnigan Trace-GC-Ultra gas
chromatograph (Thermo Fischer Scientific, Waltham, MA, USA),
equipped with flame ionization detector (GC-FID) and 2560 Capillary
GC Column (100 m, 0.25 mm diameter). Gas flow rates were 6.5 mL/min
for carrier gas (H2); 30 mL/min for the auxiliary gas (N2); 30 mL/min for
H2; and 250 mL/min for synthetic flame air. The sample division ratio
was 90 : 10. The operating parameters were established after checking
the best resolution conditions. The injector and detector temperatures
were 250 and 280 ◦ C, respectively. The column temperature was pro­
grammed at 140 ◦ C for 10 min, followed by a first ramp of 15 ◦ C/min
until reaching 200 ◦ C, remaining at this temperature for 1 min. The
second ramp was 10 ◦ C/min up to 230 ◦ C, remaining for 1 min at this
temperature. The third ramp was 0.4 ◦ C/min until 233 ◦ C, remaining in
this state for 3 min. The last ramp was 0.5 ◦ C/min, until it reached a
temperature of 238 ◦ C, which was maintained for 2 min. The total
analysis time was 41.50 min. The injections were performed in triplicate
and the injection volume was 1.2 μL. The peak areas of the FAMEs were
determined using ChromQuest 4.1 software (Thermo Fischer Scientific,
Waltham, MA, USA). The identification of FAMEs was performed by
comparison with the retention times of the FAME standards and the
quantification was done by the standard curves obtained from the
standardized compounds.
2.2.2.4. Antioxidant activity by the DPPH method. The antioxidant ac­
tivity of the CSp sample was determined according to the methodology
described by Byun, Kim, and Whiteside (2010), with modifications.
Briefly, an aliquot of the sample (0.1 mL) was mixed with 3.9 mL of
methanolic DPPH solution (0.06 mM). The mixture was vigorously
shaken on a tube shaker for 1 min and then allowed to stand at room
temperature and in the dark for 50 min. Absorbance was read at 515 nm
using a UV–vis spectrophotometer. The equipment was zeroed with 80
% methanol. The results were expressed as g sample/g DPPH, i. e., the
mass of sample required to scavenge 1 g of the DPPH free radical.
F. Nogueira Soares Souza et al.
2.2.2.5. Antioxidant activity by the β-carotene/linoleic acid system. The
antioxidant activity by the β-carotene bleaching method was determined
according to the methodology presented by Lopes-Lutz, Alviano,
Alviano, and Kolodziejczyk (2008), with modifications. Initially, a so­
lution containing 40 µL of linoleic acid, 600 mg of Tween 80, 20.6 mg of
β-carotene and 30 mL of chloroform was prepared. All chloroform was
then removed under reduced pressure, and 150 mL of distilled water
saturated with oxygen was added to the mixture under constant stirring.
In the test tube, 2.7 mL of this stable solution was mixed with 0.3 mL of
the ES. In the negative control tube, the ES was replaced by ethanol, and
in the positive control tube, it was replaced by the synthetic antioxidant
BHT. Following this, the absorbance was measured immediately at 470
nm. Afterward, the tubes were incubated in a water bath at 50 ◦ C for 60
min, then a second reading was done at the same wavelength. All
readings were performed in triplicate and the result was expressed as
milligrams of BHT equivalent per gram of sample (mg BHTE.g− 1).
2.2.2.6. Anthocyanin content. The determination of total anthocyanins
was performed according to the method described by Lees and Francis
(1972), with some adaptations. The anthocyanin quantification used the
molar extinction coefficient of cyanidin-3-glucoside. Briefly, 25 mL of
the ES based on ethanol and after acidification with HCl was added to 1 g
of sample, and then left to stand for 1 h at room temperature. After this
period, the sample was filtered. Following this, the filtered content was
collected in a 50 mL volumetric flask and its final volume was made up
with ES. Next, a spectrophotometer reading was performed at 535 nm.
Anthocyanin quantification was performed using Equation (2) described
below and the result expressed in milligrams of cyanidin-3-glucoside per
100 g of the sample.
(
AbsxMWxDF
) analysis.
TA = x100 (2)
ε
Where: TA = total anthocyanins expressed in mg of anthocyanin/100 g
of sample; Abs = absorbance at 535 nm; MW = molecular weight of
cyanidin-3-glucoside (449.2 g/mol); DF = dilution factor given by the
ratio between the final volume of the solution (50 mL) and the volume of
the sample aliquot; ε = molar extinction coefficient of cyanidin-3-
glucoside in ethanol acidified at 535 nm, whose value is 26.900 L.
mol− 1. cm− 1
2.2.2.7. Total phenolic content by Folin–Ciocalteu reagent. The total
phenolic content was determined by spectrophotometric analysis using
the Folin–Ciocalteu reagent (Ough & Amerine, 1988). Around 0.5 mL of
the sample (ES) and 2.5 mL of the Folin–Ciocalteu reagent (10 %) were
inserted into a test tube. The solution was homogenized and then 2 mL of
saturated sodium carbonate solution (Na2CO3) was added. After 2 h of
rest, readings were performed at 750 nm. For the blank, the ES was
replaced by distilled water. The result was expressed in milligrams of
gallic acid equivalent (mg GAE/100 g sample) from the linear equation:
y = 0.0113x + 0.058, R2 = 0.9888, in which “y” is the absorbance, and
“x” is the gallic acid concentration (mg/mL).
2.2.2.8. Phenolic profile by high-performance liquid chromatography
(HPLC). The extracts were prepared by following the methodology
described by Devi Ramaiya, Bujang, Zakaria, King, and Shaffiq Sahrir
(2013). Approximately 2.5 g of sample was used, which was homoge­
nized in 20 mL of methanol (HPLC grade 70 % v/v) for 1 h in an ul­
trasonic bath, at room temperature. The obtained extract was
centrifuged at 520 g-force for 15 min at 4 ◦ C and filtered through filter
paper with 14 µm porosity. For sample injection, the extracts were
filtered again using 0.45 µm porous membrane filters. The phenolic
compounds were identified and quantified by high-performance liquid
chromatography with diode array detection (HPLC-DAD/UV–vis) on a 5
µm C18 column (250 mm × 4.6 mm) maintained at 35 ◦ C; the mobile
phase was a methanol : water : acetic acid solution (70 : 28 : 2 % v/v) and
3
Food Chemistry 381 (2022) 132215
the flow rate was 1 mL/min. In the planning and execution of the vali­
dation, and the sequence of work performed as defined, the validation
parameters and acceptance criteria were: selectivity, linearity, working
range and linear range, quantification limit, recovery, precision and
accuracy, when applicable. Analyte recovery was estimated by ana­
lysing samples fortified with known amounts of analyte ‘spike’. Samples
were fortified with low, medium and high concentrations. The recovery
values of the phenolic compounds, the object of our study, ranged from
55 % to 98 %. The equations for determining the compounds were: y =
(7 × 109)x + 739.34, R2 = 0.9969 (mg gallic acid/100 g sample); y = (3
× 109)x − 233.23, R2 = 0.9968 (mg catechin/100 g sample); y = (7 ×
109)x − 1844.4, R2 = 0.9844 (mg chlorogenic acid/100 g sample); y =
(1 × 1010)x − 2181.2, R2 = 0.9918 (mg caffeic acid/100 g sample); and
y = (1 × 1010)x − 23.522, R2 = 0.9989 (mg vanillin/100 g sample),
where “y” represents the peak area in chromatogram and “x” is the
compound concentration.
2.3. Chocolate cake processing with CSp
The standard cake formulation was prepared based on the following
basic ingredients: wheat flour – 100 g, fresh eggs − 2, soy oil – 100 g,
milk – 150 g, refined sugar – 150 g and baking powder – 30 g. Additional
ingredients were: CSp, chocolate powder (50 % cocoa) – 100 g and
chocolate essence – 2 g.
First, milk, oil and eggs were mixed in a domestic blender. Then, the
dry ingredients, previously mixed, were added to the liquid mixture, and
the dough was mixed until complete homogenization. The dough was
placed into cake pans and put in a gas oven at 110 ◦ C for 45 min. After
baking, the products were cooled to room temperature prior to the
Five cake formulations were prepared, in triplicate: F0 = standard (0
%), that is, without CSp, and the others with 25 % (F1), 50 % (F2), 75 %
(F3) and 100 % (F4) substitution of wheat flour by CSp. These levels
were defined after preliminary tests.
2.4. Cake analysis
2.4.1. Technological properties of the cake
The technological properties of the baked cakes were analysed
following the method proposed by Lu, Lee, Mau, and Lin (2010).
2.4.1.1. Color measurements. The color parameters were determined
using a spectrophotometer CM-5 (Konica Minolta Inc), with a D65 in­
dicator light and an observer angle of 10◦ properly calibrated for the
CIE-L*a*b* system (L* = lightness; a* = redness; b* = yellowness). In
addition, C* and h◦ values (metric chroma and hue angle, respectively)
were also calculated.
2.4.1.2. Firmness and texture profile analysis (TPA). The firmness of the
cakes was evaluated by the penetration force on their surface and the
TPA inside the sample. TPA was performed by a TA.XT Plus textur­
ometer (Stable Micro Systems, Godalming, UK). The settings selected
were as follows: test speed 1.7 mm/s; 40 % deformation of the sample
height; a 22 mm cylindrical aluminium probe. For the TPA, settings
were: pre-test speed 2.0 mm/s; test speed 1.0 mm/s; post-test speed 5.0
mm/s; time between the two compressions 5 s; a 36 cylindrical
aluminium probe. The texture parameters recorded were hardness,
adhesiveness, cohesiveness, chewiness, resilience and firmness (all have
the same units [g]). The test was performed in triplicate for each sample.
2.4.1.3. Volume. The volume of the samples was determined by a
computational method in which many pictures of each cake were taken
at different positions using a digital camera (16.0 megapixels). Then, the
images were imported into the AutoCAD® 2018 program and adjusted
to 1 : 1 scale using the Scale command. Following this, the images of the
F. Nogueira Soares Souza et al. Food Chemistry 381 (2022) 132215

samples were contoured with a Polyline, and divided into two perpen­ sweet flavour, dark chocolate flavour, buttery flavour and cocoa flavour.
dicular imaginary planes. Finally, the Rotate command was applied, So that there was no mistake, the consumers were instructed that the
transforming the contours of the digital images into three-dimensional dominant taste is the one that was perceived with the greatest clarity
figures. The volume of each cake was acquired by the computational and predominance; that is, the most striking perception at a given
method applying the Properties command to the three-dimensional moment (Pineau et al., 2009). The samples (approximately 5 g) were
images. weighed and put into disposable white plastic cups encoded with three-
digit numbers. Finally, the consumers were instructed to taste and
2.4.2. Antioxidant activity of the cake evaluate each sample and to rinse their mouth with water between
The antioxidant activity of the cake was determined by the DPPH samples to minimize any residual effect.
method and by the β-carotene/linoleic acid system as described in sec­
tion 2.2.2.
2.5. Statistical analysis
2.4.3. Anthocyanin content, total phenolic content and individual phenolics
of the cake by HPLC A completely randomized design (CRD) with three treatments was
The determination of anthocyanins, total phenolic content and the used for statistical evaluation of the experiments. CRD results were then
phenolics profile by HPLC was performed as previously described for the submitted to ANOVA, followed by a means comparison by Tukey test at
analysis of CSp (section 2.2.2). 5 % significance (p < 0.05). An internal preference map was built using
SensoMaker software. To assess the results of the sensory tests, a cor­
2.4.4. Sensory tests relation matrix of the scores related to the attributes given by the con­
sumers was performed. The curves obtained by the TDS test were
smoothed and thus the chance level and the significance level were
2.4.4.1. Selection of tasters. Forty chocolate cake consumers with time
calculated. The chance level was defined as the dominant rate of an
available and without restrictions on the consumption of this product
attribute that would occur by chance. The significance level is the
were recruited. The selection of the tasters was carried out in two stages.
minimum value of a dominance rate that would probably not happen by
The first step was the basic taste identification test according to ISO
chance. The significance level was calculated using the confidence in­
8586:2012. The second stage assesses the taster’s discrimination ability
terval of a binomial proportion based on a normal approximation
through the application of triangular tests (Meilgaard & Civille, 2016).
(Pineau et al., 2009).
Thus, 15 tasters were selected (60 % women and 40 % men), aged be­
tween 20 and 40 years.
3. Results and discussion
2.4.4.2. Panel training. Sensory panel training was performed accord­
ing to Rocha et al. (2020). Initially, the tasters were familiarized with 3.1. Cocoa bean shell powder (CSp): Proximate analysis and fatty acid
the SensoMaker data collection software (version 1.91, UFLA, Lavras, profile
Brasil) (Nunes and Pinheiro, 2012) in three sessions, each lasting 1 h.
The training consisted of use of the program’s scale, how to evaluate the The proximate analysis of the CSp is highlighted in Table 1. The
samples and use of the program. The taster’s performance was evaluated results show a high content of carbohydrates, of which 61.3 % are water-
based on visual analysis of the TI and TDS curves for the ability to insoluble. The low content of soluble carbohydrates indicates high fiber
replicate a time curve of the same solution (prepetition > 0.05) and for
the ability to discriminate between two different solutions (psample < Table 1
0.30) of TI and TDS, for the ability to replicate a time curve of the same Cocoa shell powder: proximate composition and acid profile.
solution (prepetition > 0.05) and for the ability to discriminate two Proximate composition
distinct solutions (psample < 0.30). Components Results
− 1
Total acidity (g.100 g ) 11.4 ± 0.02
2.4.4.3. Acceptance test. The sensory attributes of the cake samples Moisture (g.100 g− 1) 7.63 ± 0.11
were assessed by means of an acceptance test with a nine-point hedonic Lipid (g.100 g− 1) 8.42 ± 0.78
scale, ranging from 1 (dislike extremely) to 9 (like extremely). The Protein (g.100 g− 1) 16.5 ± 0.18
Carbohydrate (g.100 g− 1) 61.8 ± 0.27
following attributes were analysed by the consumer sample group:
Soluble sugar (g.100 g− 1) 0.50 ± 0.02
appearance, texture, aroma, taste and overall liking. Principal compo­ Ash (g.100 g− 1) 5.69 ± 0.02
nent analysis (PCA) was carried out on the correlation of the mean P (% p/p) 0.55 ± 0.05
attribute scores averaged across the consumers and replicates for the K (% p/p) 1.96 ± 0.19
attributes that discriminated among the different formulations; finally, Ca (% p/p) 0.09 ± 0.02
Mg (% p/p) 0.65 ± 0.07
an internal map was built, which lists the scores given by the consumers
S (% p/p) 0.19 ± 0.02
for each of the attributes for the five formulations, allowing identifica­ B (ppm) 32.0 ± 1.66
tion of the intensities of the attributes, as well as the degrees of Cu (ppm) 29.2 ± 2.83
preference. Mn (ppm) 36.2 ± 4.16
Zn (ppm) 66.5 ± 7.03
Fe (ppm) 132.0 ± 15.76
2.4.4.4. Descriptive analysis Acid profile
2.4.4.4.1. Temporal dominance of sensations (TDS). TDS analysis Fatty acid Retention time % Area
was conducted according to Pineau et al. (2009), using the SensoMaker Miristic acid (C 14:0) 17.1 0.11
Palmitic acid (C16:0) 20.6 28.0
data acquisition program (Nunes & Pinheiro, 2012), under the following
Palmitoleic acid (16:1) 21.8 0.22
conditions: 40 s of analysis with a ‘delay time’ of 2 s. These conditions Margaric acid (C 17:0) 22.2 0.21
were determined by a leading group, considering the time spent by each Estearic acid (C 18:0) 24.0 34.7
consumer to evaluate a cake sample. Before carrying out the analysis, Oleic acid (C 18:1) 25.0 32.1
the consumers were trained to familiarize themselves with the TDS Linoleic acid (C 18:2) 26.4 3.21
Arachidonic acid (C 20:0) 27.4 1.03
methodology and with the sensory test. From then on, they evaluated
Behenic acid (C 22:0) 29.8 0.28
the samples in terms of the following attributes, in triplicate: sandiness, Lignoceric acid (C 24:0) 32.6 0.15

4
F. Nogueira Soares Souza et al. Food Chemistry 381 (2022) 132215

content in the residue. Martin-Cabrejas, Valiente, Esteban, and Molla
(1994), reported that cocoa shell is rich in dietary fiber, mainly con­
sisting of cellulose, carbohydrates and pectic polysaccharides. Among
the compounds that make up these fibers are lignin, cellulose and
hemicellulose. Carvalho et al. (2008), found a total carbohydrate con­
tent of 69.2 % and 25.7 % of non-fibrous carbohydrates (starch, sugars
and pectins), with fiber in neutral detergent 48.5 %, and fiber in acid
detergent 40.0 % (lignin content 17.9 %, cellulose 23.1 % and hemi­
cellulose 8.5 %). Other studies showed values for total non-starch
polysaccharide ranged from 39.9 to 55.5 %, with soluble dietary fiber
ranging from 13.1 to 41.2 % and insoluble fiber ranging from 24.2 to
42.3 % (Collar et al., 2009; Redgwell et al., 2003; Rojo-Poveda et al.,
2019). This is a favorable factor for the products elaboration in view of
the nutritional benefits associated with the addition of fiber in the
constitution of foods. Insoluble fibers have a high water retention ca­
pacity, thus improving the nutritional properties of foods without
altering the natural texture and the sensory quality of the products.
The sample also presented minerals that should be consumed daily.
For some of them, the content was similar and, in some cases, even
higher than the reference daily intake (RDI, 2016), such as: Mg: 420 mg,
P: 700 mg, Cu: 1250 µg, Fe: 18 mg, Mn: 2.3 mg and Zn: 11 mg. The
consumption of foods rich in minerals is essential, but when ingested
above their daily recommended amount, minerals can cause unwanted
side effects such as nausea, anemia, hypertension, vomiting and others.
Thus, product formulations based on cocoa bean shells must be prepared
considering the high amounts of these microminerals that may be pre­
sent in the residue.
Martínez et al. (2012) have reported similar results to those obtained
in the present investigation for the proximate composition of CSp:
moisture content of 77 ± 1 g/kg, protein content of 150 ± 2 g/kg, lipid
content of 20.2 ± 0.3 g/kg, carbohydrate content of 178.0 ± 0.9 g/kg
and ash content of 73 ± 1 g/kg. As with the cocoa bean, the composition
of the CSp depends, in addition to other factors, on its origin and the
processing to which it is submitted (Okiyama et al., 2017).
The fatty acid profile (Table 1) showed, in general, long-chain
saturated fatty acids, with emphasis on palmitic (C16:0), stearic
(C18:0) and oleic (C18:1) acids. According to Okiyama et al. (2017), the
roasting temperature can influence the CSp fatty acid profile as it can
cause the hydrolysis of triacylglycerols. When comparing the fatty acid
profile of cocoa bean shell with wheat flour, the literature demonstrates
that both profiles are similar, especially regarding the presence of the
palmitic acid (Macmurray & Morrison, 1970; Melis, Foubert, & Delcour,
2021; Prabhasankar & Haridas Rao, 1999).
3.2. Cocoa bean shell powder (CSp): Phenolic content and antioxidant
activity
From Table 2, it can be seen that the CSp contains phenolic com­
pounds which are represented by anthocyanins, in addition to gallic and
caffeic acids.
In general, several factors can interfere with the antioxidant capacity
of a sample. Therefore, in order to obtain reliable results, more than one
test must be performed to take into account different mechanisms of
antioxidant action (Schinella et al., 2010).
The results showed positive values regarding the ability of the
sample to scavenge the DPPH free radical and also regarding protection
against the oxidation of β-carotene.
Martínez et al. (2012) evaluated the antioxidant capacity of CSp
extracts obtained with different solvents and, as in the present study,
noticed their antioxidant capacity. According to these authors, antioxi­
dant capacity may be associated with the presence of phenolic com­
pounds. Lecumberri et al. (2007) observed the presence of phenolic
compounds (soluble polyphenols and tannins) and associated the anti­
oxidant capacity exhibited by CSp samples with these compounds.
Thence, the antioxidant capacity observed in our study may be directly
related to the presence of phenolic compounds.
In sum, CSp exhibited adequate chemical characteristics to be used
as an ingredient in bakery dough formulations. The high content of
insoluble carbohydrates in the samples is noteworthy, as is their anti­
oxidant capacity due to the presence of phenolic compounds, which can
provide functional properties to the products to be developed.
3.3. Cake: Phenolic compounds and antioxidant activity
From Table 2, it can be seen that the higher the percentage of CSp,
the higher the content of phenolics and anthocyanins. This behaviour
was expected as CSp had exhibited these compounds.
The anthocyanin content in the cake was substantially lower
compared to CSp. This was expected, since anthocyanins are highly
unstable at high temperatures like those used in cake manufacture
(Patras, Brunton, O’Donnell, & Tiwari, 2010). At high temperatures,
anthocyanins are hydrolysed and form aglycones, which can be trans­
formed into a chalcone structure. These compounds may be degraded to
phenolic acids spontaneously, or else polymerized with polyphenols,
leading to the formation of brown-coloured compounds (Oracz,
Nebesny, & Żyżelewicz, 2015). When analysing the different formula­
tions, it is noticed that the greater the amount of CSp, the greater the
anthocyanin content.
Studies developed by Bruna, Eichholz, Rohn, Kroh, and Huyskens-
Keil (2009) reported that products and by-products obtained from CSp
contain a large amount of phenolic compounds and prove to be a rich
and inexpensive source of compounds with an antioxidant effect. This
effect was proven in the present work, where the highest values of
antioxidant activity by DPPH and by the β-carotene/linoleic acid system
were achieved for sample F5, where 100 % of wheat flour was replaced
by CSp.
The ability to capture the free radical DPPH may also be related to
the presence of gallic acid, catechin, caffeic acid and vanillin, also evi­
denced in the study. This evaluation proves that the antioxidant capacity
found in the CSp was maintained even after the technological processes
for making the cake. Therefore, it can be stated that the replacement of
wheat flour by CSp in the development of a cake is an innovative and

Table 2
Cocoa shell powder and Cake: antioxidant activity, total anthocyanin content, total phenolic content, and phenolic profile.
Analyze Cocoa Shell Powder Samples of cakes

F0 F1 F2 F3 F4

DPPH (g/g) 47.9 484 252 195 100 62

β-carotene/linoleic acid (mg BHTE.g− 1) 93.6 78 87 90 92 96
Folin-Ciocalteu (mg GAE/100 g) 95.0 124 92 98 92 96
Total antochyanin content (mg/100 g) 4.70 2.71 4.67 6.02 7.80 8.37
Phenolic compound
6 7 6 6 6 6
Gallic acid (mg/100 g) 2.02×10− 8.91×10− 2.02×10− 2.79×10− 5.10×10− 4.85×10−
5 6 6
Catechin (mg/100 g) nd 1.10×10− 6.26×10− 4.42×10− __ __
4 5 4 4 4 4
Caffeic acid (mg/100 g) 1.57×10− 3.48×10− 1.07×10− 1.96×10− 2.87×10− 2.67×10−
6 6 6 6 6
Vanillin (mg/100 g) nd 2.12×10− 1.83×19− 1.98×10− 2.04×10− 1.89×10−

F0 = 0 % (control sample), F1 = 25 % CSp, F2 = 50 % CSp, F3 = 75 % CSp, and F4 = 100 % CSp. Nd, nondetermined, DPPH = 2,2-diphenyl-1-picrylhydrazil.

5
F. Nogueira Soares Souza et al. Food Chemistry 381 (2022) 132215

promising alternative for promoting a bioactive product.
3.4. Cake: Technological properties
The results of TPA, firmness, volume and colour of the cake samples
developed with different concentrations of CSp are presented in Table 3.
From Table 3, it can be noted that the substitution of wheat flour by
CSp did not influence the volume of the formulations. The volume of a
baked cake is a measure of its size and is represented by the amount of
air initially entrapped during mixing, in addition to the amount of
moisture, carbon dioxide and air entrapped and expanded during the
baking process (Zhou, Faubion, & Walker, 2011). It was expected that
cakes with a greater amount of wheat flour would have a higher volume
due to the technological properties inherent to this flour. However,
possible failures in the processing steps, such as the beating and cooking
steps, caused the formulations containing higher concentrations of
wheat flour to have an embattled aspect, i.e., high moisture content and
little aeration. In contrast, the presence of CSp did not hinder the
growth, possibly because the final volume of a baked cake does not only
depend on the initial air incorporated in the cake dough, but also on its
air-holding capacity during baking, as reported by Zhou et al. (2011).
TPA allows us to evaluate the parameters of the internal structure of
cakes (Esteller, Amaral, & Lannes, 2004). The firmness (hardness) of a
baked cake is related to its density (indirectly to its volume); adhe­
siveness is defined as the negative force area obtained in the interval
between the first and the second bite, that is, the force exerted by the
baked cake on the probe, holding it and preventing its return to its initial
position after the first compression; cohesiveness expresses the internal
resistance of the cake structure; chewiness denotes the amount of energy
required to disintegrate a food to a state ready for swallowing, and
resilience expresses the proportion of recoverable energy as the first
compression is relieved (Mau, Lee, Chen, & Lin, 2017).
The samples containing CSp were less cohesive than the control,
indicating that the incorporation of cocoa bean shell makes the cakes
slightly more prone to disintegration. The results showed that chewiness
was not influenced by the addition of CSp. On the other hand, the
cohesiveness and resilience of the control samples differed from those of
samples with CSp.
Table 3 illustrates the values of the colour parameters. For L*, there
was a statistically significant difference between the samples (p < 0.05).
In addition, their values being <50 indicates that all samples were
turning darker (Cohen & Jackix, 2005). Regarding the chromaticity
parameters (a* and b*), the samples exhibited brown colouring due to
their positive values for these coordinates. According to Padilha et al.
(2010), the combination of positive values for a* and b* results in a
brown colour typical of chocolate and its derivatives. For C and H, it is
observed that the addition of CSp promoted a difference in the colour of
the samples compared to the control sample with 100 % wheat flour.
In general, cakes with CSp showed a lighter brown colour than the
control sample. The cocoa bean shell colour and non-enzymatic
browning (Maillard reaction and caramelization) can influence the
final cake colour. Since the only difference between the formulations is
wheat flour, its chemical composition and transformations may have
accentuated the browning of the control cake samples.
Padilha et al. (2010) observed that the addition of yacon flour in the
formulation of chocolate cakes interfered with their chromatic charac­
teristics. Mau et al. (2017) developed chiffon cakes by replacing wheat
flour with black rice flour and found that the colour of the cake crust was
affected by the substitution. These studies, as well as our findings,
suggest that the use of an alternative to wheat flour in the formulation of
a cake tends to significantly interfere with its colour.
3.5. Sensory analysis
3.5.1. Descriptive analysis – temporal dominance of sensations (TDS)
The TDS curves demonstrate the dominance of sensory attributes as a
function of time, for each formulation (Fig. 1). The analysis shows that
there was variation in the sensory profile during the consumption of the
samples. The perceived attributes were sandiness, sweet taste, dark
chocolate flavour, buttery flavour and cocoa flavour. The buttery and
sweet attributes were predominant in the control samples and in the F1
samples. The buttery flavour was predominant from 5 to 10 s, for F0, and
the sweet taste was predominant from 5 to 15 s, for F1. The attributes of
cocoa flavour and dark chocolate were perceived by consumers in for­
mulations that contained 50 % and 75 % CSp, F2 and F3, respectively,
from 15 to 25 s for cocoa flavour (sample F2), and from 12 to 22 s for the
taste of dark chocolate (sample F3). Moreover, the attribute of sandiness
in F3 was also noticed at a time of 23 s, while in sample F4, with 100 %
CSp, the attributes identified were sandiness (5 to 10 s) and dark
chocolate flavour (10 to 25 s).
The TDS made it possible to assess the sensory difference between
the samples. For the five formulations, it was observed that an increase
in CSp concentration interfered in the perception of the attributes. Other
researchers have used the TDS technique to assess the sensory modifi­
cation of food products (Meillon, Urbano, & Schlich, 2009). The great
advantages of TDS are the short training period and the possibility to
evaluate several attributes at the same time. However, given the fact
that different consumer groups provide different descriptions about the
temporal domain of sensations (Rodrigues et al., 2016), these studies
could present a different result if another consumer group were chosen.
3.5.2. Acceptance test
The internal preference mapping for the five cake formulations and
for appearance, aroma, flavour, texture and overall impression is shown

Table 3
Technological properties of the cake.
Parameter Samples ANOVA

F0 F1 F2 F3 F4 F p-value

Volume (cm3) 89.8ª 86.9a 87.9ª 88.1a 88.7ª 0.37 0.8240

Hardness (g) 1322ª 1760ab 2464bc 3035c 2960c 16.4 0.0002
Adhesiveness (g/s) − 2.88ª − 31.3a 2.81ª − 0.72a − 1.28ª 1.49 0.2757
Cohesiveness 0.42c 0.30b 0.24ª 0.22a 0.21ª 71.4 2.57×10− 7

Chewing (g) 369ª 347a 274ª 246a 229ª 1.66 0.2359

Resilience 0.13b 0.08a 0.07ª 0.06a 0.06ª 40.6 3.75×10− 6

Firmness 622ª 737ab 1091b 1555c 1624c 26.3 2.75×10− 5

L* 29.7ab 27.6a 29.4ab 31.2b 31.1b 4.71 0.0214

a* 7.07b 4.82a 4.74ª 4.55a 4.22a 34.1 8.38×10− 6

b* 6.28c 3.57ab 3.80b 3.49ab 3.00a 78.4 1.64×10− 7

C 9.49c 6.00b 6.08b 5.74ab 4.84ª 56.3 8.02×10− 7

H 41.7c 36.6ab 38.7b 37.4ab 35.3ª 18.0 0.0001

F0 = 0 % (control sample), F1 = 25 % CSp, F2 = 50 % CSp, F3 = 75 % CSp, and F4 = 100 % CSp. L*= lightness, a*= red, b*= yellow, C = saturation e H = hue.
Same letters in the same line indicate no significant difference (p < 0.05).

6
F. Nogueira Soares Souza et al.
Fig. 1. Cake: Temporal Dominance of Sensations (TDS) results. F0 = 0 % (control sample), F1 = 25 % CSp, F2 = 50 % CSp, F3 = 75 % CSp, and F4 = 100 % CSp.
in Fig. 2. The consumers are represented by vectors that indicate the
direction of preference for each, that is, the consumers are located close
to the region of the samples they preferred. Those who are positioned in
the central region did not differentiate the samples in relation to the
evaluated attributes.
For appearance, the two principal components explained 58.42 % of
the variance in acceptance between the five cake formulations. The
spatial separation of the five formulations suggests that there is a dif­
ference in the degree of acceptance between the cakes in relation to
appearance. Most consumers preferred formulation F0 and did not
identify differences between F1 and F3.
Regarding the aroma, the first principal component (PC1) explained
42.27 % and the second principal component (PC2) explained 23.77 %
of the variance of the acceptance data. It is observed that F2 and F3 are
very close together, indicating that they did not differ in terms of
acceptance. Most consumers preferred F4 and only a small group
preferred F0.
For the flavour attribute, PC1 represented 41.30 % and PC2 27.40 %
of the total variance of the acceptance data. Formulations F1, F2 and F3
7
Food Chemistry 381 (2022) 132215
were considered similar by consumers in terms of taste. A concentration
of consumers can be seen at the bottom, indicating greater acceptance
for F1, F2 and F3. A small group of consumers negatively correlated with
PC1 gave higher scores for F0, and formulation F4 was less accepted.
For the texture attribute, PC1 explained 47.32 % and PC2 explained
22.75 % of the variance. By the arrangement of the five formulations in
the chart, the formation of three distinct groups is noted: consumers
negatively correlated with PC1 and positively with PC2 preferred for­
mulations F0 and F1; consumers positively correlated with PC1 and
negatively with PC2 considered F2 and F3 to be the most widely
accepted; formulation F4 was the least accepted.
For overall liking, both principal components explained 72.43 % of
the data variation. The spatial position suggests the formation of three
distinct groups with different degrees of acceptance: F1, F2 and F3 were
considered similar and the most accepted samples; a small group
negatively correlated with PC1 and positively with PC2 assigned higher
scores for F0; F4 showed less acceptance.
In general, it was possible to observe that consumers did not identify
differences between samples F1, F2 and F3. On the other hand,
F. Nogueira Soares Souza et al.
Fig. 2. Cake: internal preference map. F0 = 0 % (control sample), F1 = 25 % CSp, F2 = 50 % CSp, F3 = 75 % CSp, and F4 = 100 % CSp.
significant differences were noticed in sample F4, the only one with 100
% CSp. The high fibre content of the cocoa bean shell negatively influ­
enced the attributes of texture and appearance. This fact also interfered
with the technological properties of the cake, causing this formulation to
have a lower acceptance rate. Therefore, the consumers’ preference for
samples F1, F2 and F3, compared to the control sample, indicates the
feasibility of applying CSp in the manufacture of cakes.
The use of substitutes for wheat flour aims not only to provide
products with improved physical, bioactive and nutritional properties,
but mainly to meet the high demand from gluten-intolerant consumers.
Mau et al. (2017) obtained a successful formulation of chiffon cakes with
partial replacement of wheat flour with black rice powder. Morais,
Souza, Sassi, Moreira, and Maciel (2017) stated that the preparation of
pumpkin cake with chocolate based on rice flour is a viable alternative.
de Barros et al. (2020) developed cookies enriched with cocoa bean
shell, soy and green banana flour and obtained products with a high
fibre content and high content of bioactive compounds and antioxidant
activity, as observed in the present study.
4. Conclusions
The CSp had high content of insolubles carbohydrates (fibers),
minerals, different fatty acids and antioxidants, providing a functional
character to the cakes.
The gradual increase in the percentage of powder in the cakes
resulted in formulations with different technological and sensory char­
acteristics. The proportion of up to 75 % CSp provided cakes with both
satisfactory technological properties and high consumer acceptance.
This finding indicates that the use of CSp for cake production, under the
8
Food Chemistry 381 (2022) 132215
conditions of this research, is viable from the tecnological, antioxidant,
and sensory points of view.
CSp showed to be a viable substitute ingredient to be used promis­
ingly in the food industry. In addition, the use of CSp as a substitute for
wheat flour contributes to the reduction of the environmental impacts
caused by the agro-industrial residues from cocoa processing.
CRediT authorship contribution statement
Fabíola Nogueira Soares Souza: Methodology, Investigation,
Writing – original draft. Suellen Rocha Vieira: Investigation. Marina
Leopoldina Lamounier Campidelli: Investigation. Renata Abadia
Reis Rocha: Investigation. Leonardo Milani Avelar Rodrigues:
Methodology, Investigation. Pedro Henrique Santos: Writing – original
draft. João de Deus Souza Carneiro: Supervision. Iasnaia Maria de
Carvalho Tavares: Validation, Writing – review & editing. Cristiane
Patrícia de Oliveira: Conceptualization, Project administration, Re­
sources, Writing - review & editing.
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.
Acknowledgments
The authors would like to thank the Research Support Foundation of
the State of Bahia - FAPESB [Grant number BOL00422/2016] for the
F. Nogueira Soares Souza et al. Food Chemistry 381 (2022) 132215

financial support, and to the cocoa producers in the city of Ilhéus - BA - Lessa, O. A., de Carvalho Tavares, I. M., Souza, L. O., Tienne, L. G. P., Dias, M. C.,
Tonoli, G. H. D., … Franco, M. (2021). New biodegradable film produced from cocoa
Brazil for their raw material donation. Special thanks are also for the
shell nanofibrils containing bioactive compounds. Journal of Coatings Technology and
reviewers and the academic editor office members, for their accurate Research, 18(6), 1613–1624. https://doi.org/10.1007/s11998-021-00519-4
reading and insightful comments that led to an improved manuscript. Lopes-Lutz, D., Alviano, D. S., Alviano, C. S., & Kolodziejczyk, P. P. (2008). Screening of
This work is linked to a project approved by the Ethics Council and is chemical composition, antimicrobial and antioxidant activities of Artemisia essential
oils. Phytochemistry, 69(8), 1732–1738. https://doi.org/10.1016/j.
registered on Plataforma Brasil under the protocol number: phytochem.2008.02.014
70105917.5.1001.5578. Lu, T.-M., Lee, C.-C., Mau, J.-L., & Lin, S.-D. (2010). Quality and antioxidant property of
green tea sponge cake. Food Chemistry, 119(3), 1090–1095. https://doi.org/
10.1016/j.foodchem.2009.08.015
Authors’ contributions Macmurray, T. A., & Morrison, W. R. (1970). Composition of wheat-flour lipids. Journal
of the Science of Food and Agriculture, 21(10), 520–528. https://doi.org/10.1002/
jsfa.2740211008
All authors approved the final article. Mancini, G., Papirio, S., Lens, P. N. L., & Esposito, G. (2016). Effect of n
-methylmorpholine-n-oxide pretreatment on biogas production from rice straw,
References cocoa shell, and hazelnut skin. Environmental Engineering Science, 33(11), 843–850.
Malavolta, E., Vitti, G. C., & Oliveira, S. A. (1997). Avaliação do estado nutricional das
plantas: princípios e aplicações (2nd ed.). Potafos.
AOAC. Association of official Analytical Chemists. (2010). Official methods of analysis.
Martin-Cabrejas, M. A., Valiente, C., Esteban, R. M., & Molla, E. (1994). Cocoa hull: a
(20th ed.). Arlington.
potential source of dietary fibre. Journal of the Science of Food and Agriculture, 66,
Panak Balentić, J., Ačkar, Đ., Jokić, S., Jozinović, A., Babić, J., Miličević, B., …
307–311. https://doi.org/10.1002/jsfa.2740660307
Pavlović, N. (2018). Cocoa Shell: A By-Product with Great Potential for Wide
Martínez, R., Torres, P., Meneses, M. A., Figueroa, J. G., Pérez-Álvarez, J. A., & Viuda-
Application. Molecules, 23(6), 1404. https://doi.org/10.3390/molecules23061404
Martos, M. (2012). Chemical, technological and in vitro antioxidant properties of
Barišić, V., Stokanović, M. C., Flanjak, I., Doko, K., Jozinović, A., Babić, J., … Ačkar, Đ.
cocoa (Theobroma cacao L.) co-products. Food Research International, 49(1), 39–45.
(2020). Cocoa Shell as a Step Forward to Functional Chocolates—Bioactive
https://doi.org/10.1016/j.foodres.2012.08.005
Components in Chocolates with Different Composition. Molecules, 25(22), 5470.
Mau, J. L., Lee, C. C., Chen, I. P., & Lin, S. D. (2017). Physicochemical, antioxidant and
https://doi.org/10.3390/molecules25225470
sensory characteristics of chiffon cake prepared with black rice as replacement for
de Barros, H. E. A., Natarelli, C. V. L., de Carvalho Tavares, I. M., de Oliveira, A. L. M.,
wheat flour. LWT - Food Science and Technology, 75, 434–439. https://doi.org/
Araújo, A. B. S., Pereira, J., … Franco, M. (2020). Nutritional clustering of cookies
10.1016/j.lwt.2016.09.019
developed with cocoa shell, soy, and green banana flours using exploratory methods.
Meillon, S., Urbano, C., & Schlich, P. (2009). Contribution of the Temporal Dominance of
Food Bioprocess and Technology, 13(9), 1566–1578. https://doi.org/10.1007/s11947-
Sensations (TDS) method to the sensory description of subtle differences in partially
020-02495-w
dealcoholized red wines. Food Quality and Preference, 20(7), 490–499. https://doi.
Barros, H. E. A., Natarelli, C. V. L., Abreu, D. J. M., Oliveira, A. L. M., Lago, R. C.,
org/10.1016/j.foodqual.2009.04.006
Dias, L. L.d. C., … Vilas Boas, E. V.d. B. (2021). Application of chemometric tools in
Meilgaard, M., Civille, G. V., & Carr, B. T. (2016) Sensory evaluation techniques. (5th ed.).
the development of food bars based on cocoa shell, soy flour and green banana flour.
Boca Raton.
International Journal of Food Science & Technology, 56(10), 5296–5304. https://doi.
Melis, S., Foubert, I., & Delcour, J. A. (2021). Normal-Phase HPLC-ELSD to Compare
org/10.1111/ijfs.v56.1010.1111/ijfs.15127
Lipid Profiles of Different Wheat Flours. Foods, 10, 428. https://doi.org/10.3390/
Bruna, C., Eichholz, I., Rohn, S., Kroh, L. W., & Huyskens-Keil, S. (2009). Bioactive
foods10020428
compounds and antioxidant activity of cocoa hulls (Theobroma cacao L.) from
Morais, J. S., Souza, B. L., Sassi, K. K. B., Moreira, R. T., & Maciel, J. F. (2017).
different origins. Journal of Applied Botany and Food Quality, 83, 9–13.
Composição química e perfil de textura de bolo de abóbora com chocolate à base de
Byun, Y., Kim, Y. T., & Whiteside, S. (2010). Characterization of an antioxidant polylactic
farinha de arroz. Revista Brasileira de Agrotecnologia, 7, 78–81.
acid (PLA) film prepared with a-tocopherol, BHT and polyethylene glycol using film
Nunes, C. A., & Pinheiro, A. C. M. (2012) SensoMaker. (1st. ed). UFLA.
cast extruder. Journal of Food Engineering, 100, 239–244.
Okiyama, D. C. G., Navarro, S. L. B., & Rodrigues, C. E. C. (2017). Cocoa shell and its
Carvalho, G. G. P., Garcia, R., Pires, A.J.V., Pereira, O. G., Fernandes, F. E. P., Cecon, P.R.
compounds: Applications in the food industry. Trends in Food Science & Technology,
& Azevêdo, J.A. G. (2008). Fracionamento de proteínas de silagem de capim-elefante
3, 103–112. https://doi.org/10.1016/j.tifs.2017.03.007
emurchecido ou com farelo de cacau. Ciência Animal Brasileira, 9 (3), 648 - 656.
Oracz, J., Nebesny, E., & Żyżelewicz, D. (2015). Changes in the flavan-3-ols,
Cohen, K. O., & Jackix, M. N. H. (2005). Study of cupuassu liquor. Food Science and
anthocyanins, and flavanols composition of cocoa beans of different Theobroma
Technology, 25, 182–190. https://doi.org/10.1590/S0101-20612005000100030
cacao L. groups affected by roasting conditions. European Food Research and
Collar, C., Rosell, C. M., Muguerza, B. & Moulay L. (2009). Breadmaking Performance
Technology, 241(5), 663–681. https://doi.org/10.1007/s00217-015-2494-y
and Keeping Behavior of Cocoa-soluble Fiber-enriched Wheat Breads. Food Science
Ough, C. S., & Amerine, M. A. (1988). Methods for analysis of musts and wines (2nd ed.).
Technology International, 15(1), 0079–87. https://doI: 10.1177/1082013208102643.
John Wiley & Sons.
Sales de Menezes, L. H., Carneiro, L. L., Maria de Carvalho Tavares, I., Santos, P. H.,
Padilha, V. M., Rolim, P. M., Salgado, S. M., Livera, A. S., Andrade, S. A. C., &
Pereira das Chagas, T., Mendes, A. A., … Rangel de Oliveira, J. (2021). Artificial
Guerra, N. B. (2010). Sensorial profile of chocolate cakes formulated with yacon
neural network hybridized with a genetic algorithm for optimization of lipase
flour (Smallanthus sonchifolius). Food Science and Technology, 30, 735–740. https://
production from Penicillium roqueforti ATCC 10110 in solid-state fermentation.
doi.org/10.1590/S0101-20612010000300026
Biocatalysis Agricultural Biotechnology, 31, 101885. https://doi.org/10.1016/j.
Patras, A., Brunton, N. P., O’Donnell, C., & Tiwari, B. K. (2010). Effect of thermal
bcab.2020.101885
processing on anthocyanin stability in foods; mechanisms and kinetics of
Esteller, M. S., Amaral, R. L., & Lannes, S. C. S. (2004). Effect of sugar and fat replacers
degradation. Trends in Food Science & Technology, 21(1), 3–11. https://doi.org/
on the texture of baked goods. Journal of Texture Studies, 35, 383-393. https://doi.
10.1016/j.tifs.2009.07.004
org/10.1111/j.1745-4603.2004.tb00602.x.
Pineau, N., Schlich, P., Cordelle, S., Mathonnière, C., Issanchou, S., Imbert, A., …
Ferrão-Gonzales, A. D., Vital, A. V. D., Lima, J. M., & Rodrigues, M. B. S. (2013).
Köster, E. (2009). Temporal Dominance of Sensations: Construction of the TDS
Desenvolvimento sustentável para o resgate da cultura do cacau baseado no
curves and comparison with time–intensity. Food Quality and Preference, 20(6),
aproveitamento de resíduos. Interfaces Científicas-Saúde e Ambiente, 1(2), 41–52.
450–455. https://doi.org/10.1016/j.foodqual.2009.04.005
Handojo, L., Triharyogi, H., & Indarto, A. (2019). Cocoa bean shell waste as potential raw
Prabhasankar, P., & Haridas Rao, P. (1999). Lipids in Wheat Flour Streams. Journal of
material for dietary fiber powder. International Journal of Recycling of Organic Waste
Cereal Science, 30(3), 315–322. https://doi.org/10.1006/jcrs.1999.0289
in Agriculture, 8(S1), 485–491. https://doi.org/10.1007/s40093-019-0271-9
Devi Ramaiya, S., Bujang, J. S., Zakaria, M. H., King, W. S., & Shaffiq Sahrir, M. A.
Hodge, J. E., & Hodfreiter, B. R. (1962). Determination of reducing sugars and
(2013). Sugars, ascorbic acid, total phenolic content and total antioxidant activity in
carbohydrate. In: Wilster, R.C, & Wolfron, M.I. (Eds.). Methods in carbohydrate
passion fruit (Passiflora) cultivars. Journal of the Science of Food and Agriculture, 93
chemistry (pp. 380-398).
(5), 1198–1205. https://doi.org/10.1002/jsfa.2013.93.issue-510.1002/jsfa.5876
ISO 8586:2012. (2012) Sensory analysis. General guidelines for the selection, training and
Redgwell, R., Trovato, V., Merinat, S., Curti, D., Hediger, S., & Manez, A. (2003). Dietary
monitoring of selected assessors and expert sensory assessors. Retrieved from https://
fibre in cocoa shell: Characterisation of component polysaccharides. Food Chemistry,
www.iso.org/standard/45352.html. Accessed December 20, 2021.
81(1), 103–112. https://doi.org/10.1016/S0308-8146(02)00385-0
Jahurul, M. H. A., Zaidul, I. S. M., Norulaini, N. A. N., Sahena, F., Jinap, S., Azmir, J., …
Resende, L. M., Franca, A. S., & Oliveira, L. S. (2019). Buriti (Mauritia flexuosa L. f.) fruit
Omar, A. K. M. (2013). Cocoa butter fats and possibilities of substitution in food
by-products flours: Evaluation as source of dietary fibers and natural antioxidants.
products concerning cocoa varieties, alternative sources, extraction methods,
Food Chemistry, 270, 53–60. https://doi.org/10.1016/j.foodchem.2018.07.079
composition, and characteristics. Journal of Food Engineering, 117(4), 467–476.
Rocha, R. A. R., Ribeiro, M. N., Silva, G. A., Rocha, L. C. R., Pinheiro, A. C. M.,
Lecumberri, E., Mateos, R., Izquierdo-Pulido, M., Rupérez, P., Goya, L., & Bravo, L.
Nunes, C. A., & Carneiro, J.d. D. S. (2020). Temporal profile of flavor enhancers
(2007). Dietary fibre composition, antioxidant capacity and physico-chemical
MAG, MSG, GMP, and IMP, and their ability to enhance salty taste, in different
properties of a fibre-rich product from cocoa (Theobroma cacao L.). Food Chemistry,
reductions of sodium chloride. Journal Food Science, 85(5), 1565–1575. https://doi.
104(3), 948–954. https://doi.org/10.1016/j.foodchem.2006.12.054
org/10.1111/jfds.v85.510.1111/1750-3841.15121
Lees, D. H., & Francis, F. J. (1972). Standardization of Pigment Analyses in Cranberries.
Rodrigues, J. F., Souza, V. R., Lima, R. R., Carneiro, J. D. S., Nunes, C. A., &
HortScience, 7, 83–84.
Pinheiro, A. C. M. (2016). Temporal dominance of sensations (TDS) panel behavior:
Lessa, O. A., Reis, N. D. S., Leite, S. G. F., Gutarra, M. L. E., Souza, A. O., Gualberto, S. A.,
A preliminary study with chocolate. Food Quality and Preference, 54, 51–57. https://
… Franco, M. (2018). Effect of the solid-state fermentation of cocoa shell on the
doi.org/10.1016/j.foodqual.2016.07.002
secondary metabolites, antioxidant activity, and fatty acids. Food Science and
Biotechnology, 27(1), 107–113. https://doi.org/10.1007/s10068-017-0196-x

9
F. Nogueira Soares Souza et al.
Rojo-Poveda, O., Barbosa-Pereira, L., Mateus-Reguengo, L., Bertolino, M., Caroline
Stévigny, C., & Zeppa, G. (2019). Effects of Particle Size and Extraction Methods on
Cocoa Bean Shell Functional Beverage. Nutrients, 11, 867–886. https://doi.org/
10.3390/nu11040867
Schinella, G., Mosca, S., Cienfuegos-Jovellanos, E., Pasamar, M.Á., Muguerza, B.,
Ramón, D., & Ríos, J. L. (2010). Antioxidant properties of polyphenol-rich cocoa
products industrially processed. Food Research International, 43(6), 1614–1623.
https://doi.org/10.1016/j.foodres.2010.04.032
10
Food Chemistry 381 (2022) 132215
Sousa, M. S. B., Vieira, L. M., Silva, M.d. J. M.d., & Lima, A.d. (2011). Caracterização
nutricional e compostos antioxidantes em resíduos de polpas de frutas tropicais.
Ciência e Agrotecnologia, 35(3), 554–559.
Zhou, J., Faubion, J. M., & Walker, C. E. (2011). Evaluation of different types of fats for
use in high-ratio layer cakes. LWT - Food Science and Technology, 44, 8802-Zhou, J.,
Faubion, J. M., & Walker, C. E. (2011). Evaluation of different types of fats for use in
high-ratio layer cakes. LWT - Food Science and Technology, 44(8), 1802–1808.
https://doi.org/10.1016/j.lwt.2011.03.013