Temperatura-duration couples variation of cocoa beans roasting on the qualily properties of extracted cocoa butter

Annals of Agricultural Sciences 63 (2018) 19–24
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Temperature/duration couples variation of cocoa beans roasting on the
quantity and quality properties of extracted cocoa butter
T
⁎
Pauline Mounjouenpoua, , Daniel Belibib, Bongse Kari Andoseha, Alexandre Okoudab,
Kassimou Mouanfona, Eugene E. Ehabea, Robert Ndjouenkeuc
a
Institute of Agricultural Research for Development (IRAD), P.O. Box 2067, Yaoundé, Cameroon
College of Technology, University of Bamenda, Cameroon
c
National Higher School of Agricultural and Food Sciences, University of Ngaoundere, Cameroon
b
A R T I C LE I N FO
A B S T R A C T
Keywords:
Cocoa beans
Roasting conditions
Cocoa butter
Physicochemical properties
Sensorial properties
Roasting is an important process that could influence the quantity of butter extracted. Central Composite Design
(CCD) approach was used to study the influence of the couple temperature/duration of roasting on the quantity
of extracted butter. The roasting conditions used were temperatures in the range of 110–197 °C and time ranging
from 10 to 57 min. A total of 13 couple was tested. The result highlight that roasting conditions significantly
affected the quantity of obtained butter. The best couple temperature – duration were 125 °C/57 min and 140 °C/
40 min with an extraction yield of about 25%. However, obtained cocoa butter presented a wide diversity with
respect to texture, colour and odour characteristic. Physicochemical properties of extracted butter were not
function to the roasting conditions. Iodine and saponification indices were within the norms. However, the
humidity rates of the studied cocoa butter were largely above the standard rates. Findings of this research are
useful to food industries, and the impact of cocoa roasting on the extracted butter properties could help developed new products.
1. Introduction
Cocoa beans consist mainly of cocoa butter (50–55% of total mass)
which is of great socio-economic importance which is due to its physicochemical properties exploited in food processing, cosmetic, pharmaceutical and chemical industries (Kitamura et al., 2003; Maranz
et al., 2004; Schreckenberg, 2004; Żyżelewicz et al., 2014).
Roasting is one of the important step to undergo in order to extract
this healthy product as it affects its quality properties. During roasting,
aroma and flavour properties such as alcohols, pyrizines, ethers, furans,
esters, aldehydes and pyroles (Hashim et al., 1998; Jinap et al., 1998;
Misnawi and Teguh, 2010; Żyżelewicz et al., 2014) are developed at
temperatures of 110–140 °C and time range of 20–50 min (Jinap et al.,
1998).
Extraction of cocoa butter is common in rural areas of cocoa production countries and it performance varies from one region to another
due to poverty and lack of machine. Although traditional extraction
methods are largely used, extraction yields are relatively low (10–20%)
given that extraction yield depends on the degree of disruption of lipidbearing cells.
Several authors had conducted research on cocoa butter extraction
based on various parameters such as particle size of cocoa nibs, utilization of various solvent, utilization of pressure (Li and Hartland, 1992;
McHugh and Krukonis, 1994; Rossi, 1996; Asep et al., 2008).
There is no study on the optimization of cocoa roasting based on the
quantity of cocoa butter produced. This research aimed to study the
best roasting conditions which could improve butter extraction yield
using traditional extraction methods. For this study, flotation method of
cocoa extraction is used because it is the most common in cocoa areas,
compare to pressing method which is expensive. Therefore, this study
was focused on the influence of couple temperature/duration on the
quantity and the quality of butter obtained, using Central Composite
Design (CCD) with two independent variable, temperature and time and
one dependent variable, the quantity of butter as response.
2. Materials and methods
2.1. Cocoa beans
Cocoa beans (Forastero amazonian) were obtained from Bafia,
Peer review under responsibility of Faculty of Agriculture, Ain-Shams University.
⁎
Corresponding author.
E-mail address: [email protected] (P. Mounjouenpou).
https://doi.org/10.1016/j.aoas.2018.04.001
Received 8 September 2017; Received in revised form 22 March 2018; Accepted 3 April 2018
Available online 24 April 2018
0570-1783/ 2018Production and hosting by Elsevier B.V. on behalf of Faculty of Agriculture, Ain Shams University. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/BY-NC-ND/4.0/).
Annals of Agricultural Sciences 63 (2018) 19–24
P. Mounjouenpou et al.
principle of this method is based on the titration, with a solution of
sodium thiosulfate N/200, of Iodine molecules released by oxidation of
iodides by hydro-peroxides. The fat is first solubilized in a mixture of
acetic acid and chloroform.
Table 1
Central composite design for two factors and level of independent variables.
Runs
1
2
3
4
5
6
7
8
9
10
11
12
Variable in coded unit
Variable in original unit
X1
X2
Temperature: °C
X1
Duration: min
X2
−1
1
−1
1
0
0
−√2
0
0
0
0
0
1
−1
1
1
0
0
0
−√2
+√2
0
0
0
110
+140
110
140
125
125
156
125
125
125
125
125
10
10
40
40
25
25
25
14
57
25
25
25
2.4.4. Free fatty acid
The Free Fatty Acid (FFA) of butter samples were determined according to Ocho (1999) method. To extract and neutralize all the FFA
contained in butter samples, a 5 g sample of fat was dissolved in a solution of 0.01 N alcoholic NaOH in presence of phenolphthalein. The
obtained hydro-alcoholic solution was acidified with 20 ml of a 1/3
sulfuric acid solution and the liberated fatty acids were extracted with
50 ml of hexane. The excess of hexane is subsequently evaporated and
the free fatty acids are then converted to methyl esters by addition of a
methanolic solution of sulfuric acid.
2.4.5. Initial fusion point
The initial fusion point of the samples was determined by the
methods described by Hamilton and Rossel (1986).
X1, X2 = independents variables.
Centre-North cocoa production basin of Cameroon. The desired cocoa
beans were collected using a sieve. The samples were kept sealed in
bags and stored at room temperature for further analysis.
2.4.6. Humidity
Humidity of cocoa butter was determined according to the principle
of dehydration by oven drying (80 °C) of samples (5 g) until attaining of
a constant weight as described by A.O.A.C (1980).
2.2. Cocoa roasting
2.5. Sensorial characterization of cocoa butter
Roasting was carried out as suggested by the Central Composite
Design (CCD) using Design-Expert software version 6.0 (Stat Ease
Software) (Jinap et al., 1995; Montgomery, 2001). Two independent
variables were used: temperature (110–156 °C) and time (10–57 min).
The dependent variable (response) determined the quantity of the
butter extracted. The cocoa beans were roasted in an oven (BINDER:
Beiblatt-Anheben-08-06, art-Nr 7001-0123), according to variables
showed in Table 1.
Sensorial characteristics are defined according to the modified
version of sensorial test as described by Konan et al. (2003), at the Food
Technology Laboratory of the Institute of Agricultural Research for
Development, IRAD Yaoundé, Cameroon. These analysis were done by
16 trained panelists (10women and 6 men). The average age of panelist
was 33 years old for men and 27 years old for women. The sensory
analysis was conducted at room temperature (about 25 °C). The panelists were familiar with cocoa butter and were chosen for their sharpness of smell and capacity to distinguish colours. For each sample, and
for the same panelist, four repetitions were done.
2.3. Butter extraction by flotation method
Butter extraction was done according to Mounjouenpou et al.
(2012). Roasted cocoa beans were de-shelled and milled to obtain the
cake called cocoa liquor. Cocoa butter was obtained by flotation. The
cake was submerged in boiling water (about 100 °C) and the mixture
was regularly turned to allow formation of oil droplet. After that, the
floating oil droplets were collected carefully from the surface until
exhaustion. Extraction was done from 500 g of roasted cocoa.
– Texture was determined by smashing between the thumb and the
forefinger the equivalent of 1 g of cocoa butter. The butter was said
to be melting when it melted upon first friction and said to be
compact on the contrary. Scores were attributed with respect to
meltiness of butter: 1 = not, 2 = yes.
– Colour of the butter was characterized by depositing a hazel of cocoa
butter on a white sheet of paper. This feature was to evaluate how
yellow-gold the butter was presented and scores allocated were:
1 = light, 2 = moderate and 3 = intense.
– Odour was evaluated by smelling the aroma of the butter spread in
between the fingers. The smell was said to be “intense” when the
butter inhaled had the characteristic odour of roasted cocoa without
friction. The odour was said to be “moderate” if the smell was
sensed only after friction between fingers and ‘faint’ when only a
poor aroma was perceived even after friction. A three-point score
scale was used: 1 = poor, 2 = moderate and 3 = Intense.
– Taste butter samples were heated at 40 °C to make it liquid and
panelist tasted them and scores were attributed with respect to their
bitterness: 1 = bitter, 2 = not bitter.
2.4. Physicochemical analysis
2.4.1. Saponification index
The saponification index is obtained by colorimetric method according to French standard (NF ISO 3657, 2013). This method consists
of preparing the fat solution by dissolving fat in a mixed solvent
(ethanol-diethyl ether), adding when heated a solution of alcoholic
KOH, and assay the excess of KOH with a standard solution of hydrochloric acid in the presence of phenolphthalein until colorless.
2.4.2. Iodine index
The iodine index of butter samples was determined by the method
of Wijs (A.O.A.C, 1980). This method consists of treating the fatty
sample with an excess of Wijs reagent (iodine monochloride) which
binds to the double bonds. The excess reagent is dosed with potassium
iodide and the liberated iodine is assayed with sodium thiosulfate solution in the presence of starch paste.
2.6. Statistical analysis
All analyses were done in triplicate. Test of normality was used to
evaluate the distribution of data on the quantity of butter obtained.
After that, the non-parametric Kruskall-Wallis Ranking test was used to
analyze the effect of different couples of temperature – duration on the
quantity of butter produced. Linear regression was also done to confirm
the result which was illustrated by a boxplot. Statistical software used
2.4.3. Peroxyde index
The peroxide index of butters was determined by Near-Infrared
spectrometry, according to French standard (NF T 60-220, 1995). The
20
Annals of Agricultural Sciences 63 (2018) 19–24
P. Mounjouenpou et al.
oleiferous cells in order to release oil. There are many different ways to
roast cocoa beans; most of them depend on the type of derived product
that is being made. Roasting conditions and extraction method significantly influenced the quantity of butter obtained. The results of this
study indicated that high temperature – short duration and low temperature – long duration seemed to be the best roasting conditions of
cocoa beans, and proved that the quantity of butter extracted was
temperature and time dependent.
The butter extraction yield obtained using traditional extraction
method in this study (about 25%) was better than that of Adabe and
Ngo-Samnick (2014), and Ramli et al. (2008) who obtained a maximum
extraction rate of 15%, with cocoa bean roasting condition of 98–120 °C
for 90–95 min, and at 120 °C, 130 °C, 140 °C, 150 °C, 160 °C, 170 °C for
20, 30, 40, 50 min respectively. Similar results were obtained with
other vegetal butter extracted using two traditional methods (15–28%)
(Badoussi et al., 2015). Comparatively to improved method, traditional
method extraction performance was significantly lower than that of
press extraction (46%) (Adabe and Ngo-Samnick, 2014), or chemical
extraction (45.0–51.4%) (Badoussi et al., 2015).
The Shapiro-Wilk normality test revealed that the quantity of butter
extracted according to roasting condition was not normally distributed
(p-value > 0.05). Therefore the Kruskall-Wallis ranking test was used
to evaluate the effects of the different couples (temperature/duration)
on the quantity of butter produced. This test highlighted that roasted
condition (couple temperature/duration) significantly influenced the
quantity of butter obtained (Fig. 1). This result was also confirmed by a
linear regression which attested these effects, with runs 4 and 9 roasting
conditions, i.e. 140 °C/40 min and 125 °C/57 min, being the best.
Table 2
Central Composite Design (CCD) for the quantity of butter obtained from
roasted cocoa beans.
Runs
Temperature (°C)
Duration
(min)
Average quantity of
butter (g)
Extraction yield
(%)
1
2
3
4
5
6
7
8
9
10
11
12
110
140
110
140
125
125
156
125
125
125
125
125
10
10
40
40
25
25
25
14
57
25
25
25
75.1 ± 1.2
98.3 ± 0.9
98.3 ± 1.3
125.0 ± 2.7
73.3 ± 1.7
71.6 ± 1.8
109.5 ± 0.9
59.3 ± 1.8
123.9 ± 1.9
70.3 ± 1.6
69.3 ± 1.5
71.3 ± 0.9
15.0
19.6
19.6
25.0
14.6
14.3
21.9
11.9
24.8
14.1
13.9
14.3
± : Standard deviation.
are Graph pad prism (ShapiroWilk, test of normality), R.3.3.1 (KruskallWallis ranking test, linear regression and boxplot).
3. Results and discussion
3.1. Quantity of butter extracted base on the temperature-duration couple
used
Twelve roasting conditions (couple temperature/duration) were
assigned based on the Central Composite Design (CCD) results, with 5
central points with same couple temperature – duration (125 °C/
25 min). CCD for the quantity of butter obtained from the roasted cocoa
beans is shown in Table 2.
According to roasting condition, the quantity of butter extracted
from 500 g of roasted cocoa beans by traditional method ranged from
59 g to 125 g. Table 2 highlighted that the extraction yield increased
with temperature and time. The best conditions of roasting (couple
temperature/duration) observed were 125 °C for 57 min, and 140 °C for
40 min, with the highest butter quantity of 123.9 g and 125.0 g respectively. These values represented about 25% of roasted cocoa beans
mass.
Roasting is an important operation which allows bursting of
3.2. Sensorial characterization of extracted cocoa butter
Sensorial characterization of the cocoa butter obtained was done on
only 8 samples (R1, R2, R3, R4, R5, R7, R8, and R9) because the experimental design plan gave five central point (R5, R6, R10, R11, R12)
with the same couple temperature-duration (125 °C/25 min).
The quantity of cocoa butter obtained in this study presented a wide
diversity with respect to texture, colour, taste and odour.
Irrespective of the sample, taste and texture evaluations showed
that all the extracted butters were not bitter and melted in contact with
fingers.
Fig. 1. Effect of couples temperature/duration on the quantity of produced butter.
21
Annals of Agricultural Sciences 63 (2018) 19–24
P. Mounjouenpou et al.
The light golden-yellow butter (R1, R2, and R8) had iodine index
ranging from 33 to 38 gI2/100 g, peroxide index was ranged from 20.30
to 22.88 mEgO2/kg, higher saponification matters: saponification index
from 178 to 196 mg KOH/g) and FFA from 1.81 to 1.97%. Light goldenyellow butters had humidity rate of 13%.
The moderate golden-yellow butter (R3, R5) had iodine index ranging from 40 to 42 g I2/100 g, peroxide index of 18.13 to 19.28 mEgO2/
kg, saponification index of about 191 mg KOH/g, and FFA of 1.86%.
Moderate golden-yellow butters had humidity rate of 13%.
As for the cocoa butter with an intense golden-yellow coloration
(R4, R7 and R9), its iodine index was ranged from 35 to 41 gI2/100 g,
peroxide index were ranged from 33.22 to 40.24 mEgO2/kg, saponification index ranged from 177 to 190 mg KOH/g, and FFA ranged from
1.85 to 1.99%. Intense golden-yellow butters had humidity rate of 14%.
Roasting conditions contributes to many physical and chemical
changes that significantly alter their properties. Extracted cocoa butter
samples presented an important variation in physicochemical properties. This could be explained by the diversity of roasting parameters
used (Hall et al., 1996).
Iodine Value (IV) is a convenient indicator of the degree of hardness
of cocoa butter. The Iodine values of the analyzed fats ranged from 33
to 42 gl2/100 g. The lowest IV values were (29.4 and 31.9 g I2/kg).
These values were within limits laid down in the literature (Chaiseri
and Dimick, 1989; Shukla, 1995). Higher values of IV could be due to
the presence of antioxidant pigments responsible for the yellow coloration of butter (Ayeh, 1991), and also indicated a higher content of
unsaturated fatty acids including triacyclglycerols. These acids are responsible for most of its softness (Chaiseri and Dimick, 1989). Albi et al.
(1997) observed that the lowest Iodine value can be correlated to
highest values of hardness. This may be due to high temperatures of
heating in a short time, which causes unforeseen changes in the fatty
acids included in the triacylglycerols.
The peroxide index of extracted butter samples were within the
standards (inferior to 50 mEgO2/kg) (A.O.A.C, 1980), Change in the
peroxide value may be due to roasting conditions and the effects of
antioxidant substances in the cocoa butter formed during heating
(Tynek et al., 2001). It may also be the consequence of uncontrolled
conditions of drying and conservation. The relatively low obtained
peroxide value of cocoa butter was the characteristics of fat extracted
from raw cocoa beans. Tan and coworkers (Tan et al., 2001) believe
that the reasons for low values of can be found in the formation of
hydroxyperoxides at lower temperatures. However, longer heating increases the temperature, which contributes to the rapid decomposition
of the hydroxyperoxides to secondary, labile products, which can
transform into products such as alcohols, aldehydes, ketones, acids,
dimers, trimers, polymers and cyclic compounds.
The saponifiable fraction of butter samples was studied through
saponification index and Free Fatty Acid. The obtained saponification
indexes are within the limits of standards norms. According to Chaiseri
and Dimick (1989), Shukla (1995), saponification values are between
188 and 198 mg KOH/g, and the softening temperature between 30 and
34 °C. The lower saponification values may be due to the long duration
of roasting with higher temperature (Albi et al., 1997). These changes
may also probably come from the degradation of triacylglycerols and
changes in free fatty acids. Yoshida et al. (1995) found that the triacylglycerols present in vegetable oil were slightly hydrolyzed during
transformation.
FFA reflects the degradation of triglycerides. FFA levels of all butter
samples were above the standard, i.e. above 1.75%. These findings were
similar to that of Ivorian cocoa butter where important levels of FFA
were also obtained on some cocoa producer areas (Guéhi et al., 2008;
Dano et al., 2013; Kedjebo et al., 2015). Indeed, FFA provide information’s on the degradation rate of cocoa butter that can either result from an enzymatic activity, or result from the mishandling of postharvest treatments (Guéhi et al., 2010). An important FFA content
would strongly affect the fundamental technological properties of
Three levels of golden-yellow colour intensity were obtained (light,
moderate and intense) with 37.5% light, 25% moderate and 37.5%
intense golden-yellow colour.
Cocoa roasted aroma or odour was more intense at high temperature of roasting with samples R3, R4 R7 and R9, than that of R1, R2, R5,
and R8 where temperatures were lower. Three groups of cocoa butters
were obtained with respect to odour intensity (faint, moderate and
intense) with a dominance of an intense odour (50%, representing R3,
R4, R7 and R9), followed by moderate odour (R2 and R5) and faint
odour (R1 and R8).
Roasting is an important operation for the development of sensorial
properties of cocoa beans (Jinap et al., 1998). Cocoa beans that are not
roasted have a bitter, acidic, astringent, and nutty flavour (Afoakwa
et al., 2008). Several researchers had reported on the effect of cocoa
beans roasting conditions on the formation of cocoa flavour compounds
(Finken, 1996; Swiechowski, 1996; Nebesny and Rutkowski, 1998;
Misnawi et al., 2004; Ramli et al., 2008). Likewise, optimization of
roasting condition in term of flavour compounds, formation of pyrazine
and acrylamide had been studied (Farah et al., 2012; Żyżelewicz et al.,
2017). Sensorial properties are important parameters in cocoa classification. It is a result of a combination of 400–500 compounds including
aldehydes, ethers, thiazoles, phenols, sulfur compounds, pyrazines,
ketones, alcohols, furans and esters (Dimick and Hoskin, 1981; Hoskin
and Dimick, 1984).
Findings of this study points out an important sensorial diversity of
extracted cocoa butter that could be due to the diversity of extraction
methods, notably variation in roasting conditions (temperature and
roasting duration) of cocoa beans (Hall et al., 1996). This diversity in
sensorial properties has also been obtained by several researchers on
vegetable oils (Hall et al., 1996; Kitamura et al., 2003; Mbah et al.,
2005).
Flavour is the sum of perceptions resulting from stimulation of the
sense ends that are grouped together at the entrance of the alimentary
and respiratory tracks (Molnár, 2009). Ramli et al. (2008) experimented several cocoa roasting conditions on the flavour component:
and concluded that there is a linear correlation between roasting temperature and that of flavour compounds (pyrazine compound formation). Misnawi and Teguh (2010) highlighted that the formation and
the concentration of pyrizines depend on temperature and duration of
roasting conditions. Farah et al. (2012) also indicated that the concentration of pyrizines increased with temperature, from 110 °C to
160 °C but dramatically reduced when roasting time was increased.
Cocoa flavour is better developed at high temperature. As temperature
increase, there is more formation of diketopiperazines which when
mixed with theobromine, will contribute to the cocoa taste (Beckwett
and Ziegleder, 2009; Farah et al., 2012).
Colour is a quality that greatly influence the appearance of a product (Molnár, 2009) since it is the first impression that strikes the
consumer (Widodo et al., 2015). Butter samples had various colour irrespective of roasting conditions. Krysiak (2011) concluded that the
ratio of anthocyanins responsible for yellow and brown pigments in the
cocoa bean was dependent on the roasting conditions. Żyżelewicz et al.
(2014) showed the relationship between the conditions of the roasting
process, the degree of cocoa beans roasting, the content of polyphenols
and Maillard reaction products and the content of colour compounds.
Texture foodstuff relates to its roughness, smoothness, graininess as
sensed by the eyes, skin and/or mouth muscles (Molnár, 2009). Texture
of samples melted in contact with fingers. This could be attributed to
their chemical composition (high content of saturated fatty acids) as
shown by Maranz et al. (2004).
3.3. Physicochemical characterization of extracted cocoa butter
The results of the main physicochemical properties of cocoa butter
extracted from roasted cocoa beans using a Central Composite Design
are summarized in Table 3.
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Annals of Agricultural Sciences 63 (2018) 19–24
P. Mounjouenpou et al.
Table 3
Some physicochemical properties of cocoa butter samples.
R1
R2
R3
R4
R5
R7
R8
R9
Iodine index (gl/100 g)
Peroxide index (mEqO2/kg)
Saponification index (mgKOH/g)
Free fatty acid (%)
Fusion point (°C)
Humidity (%)
36
33
40
35
42
37
38
41
22.88
20.30
18.13
33.22
19.28
40.24
22.45
38.32
196
178
191
179
191
177
195
190
1.81
1.97
1.86
1.99
1.87
1.90
1.92
1.85
31
33
32
30
32
30
34
33
13
15
13
14
13
14
13
14
±
±
±
±
±
±
±
±
0.8
2.2
2.0
1.9
1.7
2.3
2.2
2.1
±
±
±
±
±
±
±
±
2.2
1.5
1.3
1.8
1.7
2.3
1.8
2.6
±
±
±
±
±
±
±
±
2.9
2.2
2.8
2.1
3.9
1.7
2.4
2.0
±
±
±
±
±
±
±
±
0.2
0.1
0.0
0.4
0.1
0.3
0.2
0.2
±
±
±
±
±
±
±
±
2.2
1.8
2.0
2.3
1.9
1.6
1.7
2.4
±
±
±
±
±
±
±
±
0.7
1.2
0.8
0.5
1.1
1.1
0.5
0.6
± : Standard deviation.
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butter. It also has an adverse effect on crystallization treatments such as
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(13–15%). The relatively high humidity rates could be linked to the use
of water for its extraction, but also for their adulteration in post-preparation with water (Hall et al., 1996). Fats exposed to air could undergo hydrolysis and oxidation reactions under the combined effects of
atmospheric germs (lipase and oxidase action), sun rays and atmospheric oxygen.
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4. Conclusion
The Central Composite Design permitted the definition of 12
roasting conditions based on the couple temperature/duration. The
cocoa butter was extracted traditionally from cocoa beans roasted according the above-mentioned conditions. According to the results obtained, extraction yield increased with temperature and time. The best
conditions of roasting observed were 125 °C for 57 min, and 140 °C for
40 min, with the highest quantity of butter: 123.9 g and 125.0 g respectively. These values represented about 25% of cocoa beans. These
roasting conditions permitted to obtain cocoa butter samples which
varied with respect to texture, odour and colour. Iodine and saponification indices were within the norms or standards. However, the humidity rates of the studied cocoa butter were largely above the standard
rates probably due to extraction in water.
Acknowledgements
All the staff of the Laboratory of Food Technology of the Institute of
Agricultural Research for Development (IRAD) is duly acknowledged.
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