Received: 19 December 2017 Revised: 10 May 2018 Accepted: 14 May 2018

DOI: 10.1111/jfpe.12825

ORIGINAL ARTICLE

Production of cocoa and carob-based drink powders by foam

mat drying
Maja Benković1 nas3 |
| Kristina Radić2 | Dubravka Vitali Čepo2 | Edvinas Jašku
Laurynas Janutis3 | Marija Morkunaite3 | Siniša Srecec4

1
Faculty of Food Technology and
Biotechnology, University of Zagreb, Zagreb,
Croatia
2
Faculty of Pharmacy and Biochemistry,
University of Zagreb, Zagreb, Croatia
3
Kaunas College, University of Applied
Sciences, Kaunas, Lithuania
4
Križevci College of Agriculture, Križevci,
Croatia
Correspondence
Maja Benković, Faculty of Food Technology
and Biotechnology, Pierottijeva 6, 10000
Zagreb.
Email: mbenkovic@pbf.hr
Funding information
Croatian Science Foundation, Grant/Award
Number: IP-11-2013-3304-TEUCLIC
Abstract
The effect of substitution of cocoa powder with carob and sucrose with stevia, on physical,
chemical, and sensory properties of powder drink mixtures was studied. These powders were
then subjected to foam mat drying to produce easily solvable instant powders and to determine
the effect of the process on their physical, chemical, and sensory characteristics. The addition of
carob flour to cocoa/sugar mixtures caused a decrease of cohesion index and mean cake
strength, which is beneficial for powder handling. Foam mat drying process led to further
improvement of physical properties. To obtain a mixture with good physical, chemical, and
sensory characteristics, only a small part of cocoa powder can be replaced by carob flour (up to
10%). Overall, the foam mat drying process leads to formulation of a product with better
physical and sensory characteristics and can be successfully applied for production of cocoa/
carob/sugar drink powders.
Practical applications
Consumer demands for newly developed foods with natural, healthy ingredients is increasing
nowadays. Carob flour represents a cheaper alternative to cocoa and due to the presence of
naturally occurring carbohydrates represents a raw material with low glycemic index and there-
fore the exploration of its utilization in instant drink powders is of great significance. On the
other hand, the industry seeks cheaper alternatives to spray drying and liophyilisation as
the wide spread processes for instant powder production. The foam mat drying process is a
simple and economical alternative to spray drying and freeze drying. The results of this study
indicate that the foam mat drying process can be successfully used in the cocoa and carob drink
powder production because it results in powders with better flow properties, which is favorable
in the powder handling industries.

1 | I N T RO D UC T I O N protective, chemo preventive, and neuroprotective properties owing to

Instant cocoa powder drink is a very popular food product present on
the market, not only among children but also among adults. Factors
owing to such popularity of cocoa based products and drink powders
are, among others, good dispersibility and solubility (Benković et al.,
2015), their unique sensory and pleasant melt-in-the-mouth properties
(Aprotosoaie, Luca, and Miron, 2016) and abundance of bioactive com-
pounds, mostly flavanols (Keen et al., 2005). Its anti-inflammatory, cardio
the bioactives abundance are well-documented (Aprotosoaie et al., 2016,
Nehling, 2013, Martin et al., 2013, Allgrove & Davison, 2014).
The use of carob powder as a cheaper cocoa or chocolate substi-
tute is continuously mentioned and explored, mostly due to its abun-
dance in carbohydrates, dietary fiber, and bioactive compounds.
Furthermore, carob is known to be a widely available crop character-
ized by low cost. Carob is usually used in foodstuffs in the form of
flour. Previous research document the presence of carbohydrates

This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium,
provided the original work is properly cited.
© 2018 The Authors. Journal of Food Process Engineering published by Wiley Periodicals, Inc.
J Food Process Eng. 2018;41:e12825. wileyonlinelibrary.com/journal/jfpe 1 of 11
https://doi.org/10.1111/jfpe.12825
2 of 11
(76%), proteins (6%), fat (2%), minerals, and bioactives in carob flour
(Yousef et al., 2013). Carob pods also contain seeds which are used
for carob bean gum production. Carob (locust) bean gum is widely
used in the food industry as a thickener (E410) which is added to
numerous dairy and confectionery products, or as a stabilizer in low
fat products (Unal et al., 2003, Yasar et al., 2009).
For instant cocoa powder drink mixes, spray drying is usually used
as a production method. Although commonly used, this method has
its downfalls. According to Barbosa-Canovas, Ortega-Rivas, Pablo,
and Hong (2005), the main disadvantages of spray drying are high
installation costs, low thermal efficiency, energy waste, and the han-
dling of powder laden air at saturated or near saturated conditions.
Foam mat drying represents an interesting alternative for applica-
tion in cocoa/carob drink powder mix production. Basic principle of
foam mat drying is conversion of a liquid or a semi-liquid foodstuff to
foam and thin layer drying of this foam. Although the industrial drying
process was complicated and required large energy consumption, it
can be simplified without the loss of final product quality. According
to Sangamithra, Venkatachalam, Swamy, and Kuppuswamy (2015) and
Kadam et al. (2010), foam mat drying is a simple and economical alter-
native to spray drying and freeze drying and the renewed foam mat
drying is considerably cheaper due to rapid drying at lower tempera-
ture, retention of nutritional quality, and easy reconstitution. Further-
more, foam mat drying is finding an increasing application in drying
liquids such as milk, fruit juices, coffee, and tea, in a commercial scale
(Bag et al., 2011). Foam-mat drying also makes it possible to obtain a
free-flowing powder from materials that have a tendency to agglom-
erate and adhere to dryer walls (Ratti and Kudra, 2006).
Therefore, the aim of this article was to determine the effect of
substitution of cocoa powder with carob and sugar with stevia, on
physical, chemical, and sensory properties of powdered drink mixes.
Furthermore, these powders were subjected to foam mat drying to
produce easily solvable powders and assess the adequacy of such pro-
cess for production of cocoa/carob powders.
2 | MATERIALS AND METHODS
2.1 | Materials
Carob pods used for carob flour production were obtained from the local
manufacturer from the island Drvenik Mali (Croatia). Carob pods were
harvested during September 2015. Pods were first ground in a hammer
mill HPM-250 (Šcukanec, Croatia) to obtain a coarse fraction, and then
subsequently in a FOSS CT 193 Cyclotec mill (Foss, Hilleroed, Denmark)
to obtain fine particle size powder (d[0.5] =80 μm), which were then
used for cocoa/carob mixture formulation.
Sucrose and cocoa powder with 10–12% fat content were
obtained from Kraš (Zagreb, Croatia). Median diameter of cocoa pow-
der used was 13.32 μm and of sucrose 847.20 μm. Maltodextrin
(Proteos, Split, Hrvatska), whey (59%) and soy protein (39%) mixture
(including emulsifier [soy lecithin], dextrose, palm oil, aroma,
anti-caking agent, metasilicic acid, and vitamin B6) (dm, Karlsruhe,
Germany), carboxymethylcellulose (Dekora, Alicante, Spain), and
BENKOVIĆ ET AL.
TABLE 1 Composition of cocoa/carob mixtures
Sample Components, % (wt/wt)
S1 10% carob + 20% cocoa + 70% sucrose
S2 20% carob + 10% cocoa + 70% sucrose
S3 30% carob + 70% sucrose
S4 10% carob + 20% cocoa + 69.7% g sucrose + 0.3% stevia
S5 20% carob + 10% cocoa + 69.7% sucrose + 0.3% stevia
S6 30% carob + 69.7% sucrose + 0.3% stevia
Control samples
K1 30% cocoa + 70% sucrose
K2 30% cocoa + 69.7% sucrose + 0.3% stevia
stevia powder (dm, Karlsruhe, Germany) with median particle size
<100 μm were all obtained from a local store.
Chemicals used for analyses were as follows: Folin–Ciocalteu
reagent (Kemika, Zagreb, Croatia), sodium carbonate anhydrous
(Na2CO3) (Gram-mol, Zagreb, Croatia), acetone 100% (Kemoplastika,
Zagreb, Croatia), ethanol 96% (Kefo, Ljubljana, Slovenija), ammonium
peroxidisulfate ([NH4]2S2O8) (Sigma Aldrich, Steinheim, Germany),
2,20 -Azinobis(3-ethylbenzothiazoline-6-sulfonic acid) diammonium salt
(ABTS), (Sigma Aldrich, Steinheim, Germany), ()-6-Hidroxy-2,-
5,7,8-tetramethylchromane-2-carboxylic acid (Trolox) (Sigma Aldrich,
Steinheim, Germany).
2.2 | Methods
2.2.1 | Preparation of the cocoa/carob powder mixtures
The base for cocoa drink mix formulation was 30% cocoa and 70%
sugar, as previously stated by Belšcak-Cvitanović et al. (2010). The
total amount of cocoa powder (30%) was then partially or completely
replaced by carob flour and the sugar was partially replaced with ste-
via. Although the sweet strength of stevia is much higher than that of
sucrose, the basis for mixture formulation remained the same for all
samples, as other components (proteins, maltodextrin) were added to
the mixtures prior to foam mat drying, which reduced the sweetness
of the foam mat dried powders. Composition of the cocoa/carob pow-
der mixtures is shown in Table 1.
Components were mixed for 10 min at 40 rpm in a Turbula mixer
(Willy A. Bachofen Maschienenfabrik, Muttenz, Switzerland) to obtain
a homogenous mixture at an ambient temperature of 18–20  C. After
mixing, samples were packed in HDPE bags and stored at ambient
conditions (18–20  C, 50% relative humidity) until further analyses.
2.2.2 | Foam mat drying
The foam mat drying process was performed based on a preliminary
experiment concerning the influence of mixture composition, mixing
time, drying time, and drying temperature on foam properties and final
product quality (data not shown). Prior to foam mat drying, whey
(59%) and soy (39%, as stated by the manufacturer) protein mixture
(5% wt/vol), maltodextrin (5% wt/vol), and carboxymethylethyl cellu-
lose (0.5% wt/vol) were added to cocoa/carob powder mixtures. The
ingredients were dry mixed and 200 ml of distilled water was added
gradually, to avoid lump formation. The mixture was homogenized
manually using a spatula and transferred to a kitchen blender (Philips,
BENKOVIĆ ET AL.
Amsterdam, Netherlands) and blended for 7 min. The density of the
foam was determined by measuring the mass of a fixed volume of the
prepared foam, while the stability was estimated by reading the vol-
ume of the prepared foam after 2 hrs at room temperature and calcu-
lated as the ratio between the final and the initial volume. Foams
were dried at 60  C for 24 hrs in a convective oven dryer at a con-
stant air velocity of 0.35 m/s. The oven dryer was equipped with a
hot air circulation blower to ensure a uniform temperature throughout
the total volume of the drying chamber (60 L). After drying, samples
were left to cool to room temperature and milled using IKA Control
Tube Mill (IKA Werke, Germany) at 15,000 rpm for 15 s to obtain a
powdered product. Powders were packed in freezer bags until further
analyses.
2.2.3 | Analysis of physical properties
Particle size distribution
Particle size distribution was analyzed by laser diffraction method.
Malvern Mastersizer 2000 equipped with a Scirocco dry dispersion
unit (Malvern, Worchestershire United Kingdom) operating at 2 bar
pressure and 70% feed rate was used to obtain median (d[0.5]) and
Sauter diameters (D[3,2]) of the original and foam mat dried mixtures.
Analyses were done in triplicate.
Bulk density
Bulk density was determined according to a modified method previ-
ously described by Haugaard Sorensen, Krag, Pisecky, and Wester-
gaard (1978) and Benković et al. (2015). Laboratory made jolting
volumeter was used to determine bulk density after 10 taps (10 taps
were used to reduce possible errors) and 100 taps. Analyses were
done in triplicate.
Moisture content
Moisture content was determined according to a standardized AOAC
gravimetric method, as the difference in mass of the original sample
and the sample dried for 3 hr at 105  C (AOAC International, 1990).
Cohesion index
Cohesion index was determined by powder rheometer method previ-
ously described by Janjatović et al. (2012). Approximately 160 ml of
sample was poured in a measuring cylinder, weighed and mounted on
the base of the TA.HD.Plus Texture Analyzer coupled with Powder
Flow Analyzer (StableMicro Systems, Godalming, United Kingdom).
During three consecutive downward movements of the blade in the
measuring cylinder, cohesion coefficient was calculated as the area
under the negative part of the force/distance curve. Cohesion index
was then obtained as the ratio between cohesion coefficient and sam-
ple weight.
Mean cake strength
Mean cake strength was also determined by Powder Flow Analyzer
(StableMicro Systems, Godalming, United Kingdom). First, cake
strength was determined as the force required to cut the cake formed
after five consecutive compression cycles, and mean cake strength
3 of 11
was then calculated by dividing cake strength value with the initial
height of the powder in the measuring cylinder.
Solubility index
Solubility index was determined according to a modified method by
Haugaard Sorensen et al. (1978). Approximately 2 g of sample was
weighed and 10 ml of water was added to the beaker containing the
sample. The mixture was stirred with a spatula for 90 s and then left
to settle for 15 min. After that, two 5-min centrifugation cycles were
performed (Hettich, Tuttlingen, Germany) at 6000 rpm. After centrifu-
gation, the volume of sediment in the centrifuge tube (ml) was read
and expressed as solubility index.
Dispersibility
Dispersibility was determined by a stirring test, as the time in seconds
taken to disperse a given amount of powder into a given amount of
water of a given temperature (Haugaard Sorensen et al., 1978). Distilled
water of 50 ml (24  C) was poured into a beaker and 5 g of sample was
added. At the same time, stop watch was started and manual stirring
began (approximately 25 circular stirring movements within 15 s). Mea-
surement was completed when all the lumps were dispersed.
2.2.4 | Analysis of chemical properties
Extract preparation
Twofold extraction of 1 g of sample was carried out with 12.5 ml of
70% acetone on a magnetic stirrer (500 rpm, 70  C, 30 min). After
extraction and centrifugation, the supernatant was recovered and the
crude residue extracted again with another 12.5 ml of 80% acetone.
The supernatants obtained from both extractions were combined, the
solvent removed by evaporation and the residue re-suspended to a
known volume with water.
Total polyphenols and antioxidant capacity
Total phenol content (TPC) of carob extracts was determined spec-
trophotometrically according to a modified method of Lachman
et al. (1998).
The Trolox equivalent antioxidant capacity (TEAC) of cocoa drinks
was estimated by the ABTS radical cation decolorization assay (Re et al.,
1999). Results were expressed as Trolox equivalents and derived from a
calibration curve determined for Trolox (100–1,000 μM).
2.2.5 | Sensory properties
Sensory properties of the formulated mixtures were evaluated according
to a hedonistic scale. Trained panelists (n = 6) were asked to evaluate
the powder, as well as the prepared drinks. Attributes evaluated for the
powder mixture (both original and foam mat dried) were: overall appear-
ance, color and odor. For the prepared drinks, overall appearance, color,
odor, sweetness and aftertaste were evaluated based on a scale in the
range of 1 to 9 (1-dislike extremely, 9 –like extremely).
2.2.6 | Data analysis and statistics
Data analysis was performed using Statistica v.10 software (StatSoft,
Tulsa, OK), conducting the least significant difference test. Samples
were treated as dependent samples and the differences were
4 of 11
TABLE 2 Foam densities and foam stabilities of the prepared cocoa/
carob foams
Sample Foam density (kg/m3) Foam stability (%)
S1 336  1.2 57.33  0.6
S2 236  2.0 47.06  0.3
S3 226  0.9 79.27  0.9
S4 277  3.3 50.00  1.1
S5 334  10.4 33.33  0.6
S6 200  2.6 58.82  0.6
Control samples
K1 343  3.2 35.53  0.2
K2 327  2.6 41.67  0.5
accepted as significant at p < .05. To find similarity patterns between
physical, chemical, and sensory properties of the samples, Principal
Component Analysis was performed using XLStat (Addinsoft SARL,
New York, NY), a Microsoft Office Excel add-in for statistical analysis
(Microsoft, Redmond, WA).
3 | RESULTS AND DISCUSSION
3.1 | Foam properties
Properties of the cocoa and carob foams are shown in Table 2.
Previous research has shown that cocoa powder particles form a
network structure with added stabilizers and proteins, which stabilizes
the mixture and increases its viscosity (Boomgaard, Vilet & Hooyi-
donk, 1987). The formation of the network happens in several stages:
first the protein binds to the cocoa particle, then the micro-coagulated
particles are formed which are finally interlocked by a stabilizer (ADM
Cocoa, 2006). The structure of the network has been partially
explained by Gallo et al. (2013) stating that the network is actually
formed between proteins and polyphenols present in the cocoa pow-
der. Besides cocoa-protein interactions, cocoa-sugar interactions have
also been documented in high viscose products which are rich in
sugar, where the cocoa- sugar interactions cause an undesired thick-
ening effect (De Muijnck, 2005). Based on data shown in Table 2, it
can be noticed that the lowest foam densities were achieved for sam-
ples with the whole content of cocoa was replaced by carob flour
(S3 and S6), and the opposite trend was visible for the foam stability
values: samples S3 and S6 made only with carob flour and sugar (and
stevia, in the case of S6) had the highest foam stability in comparison
to other samples. This was an indication that carob flour acted benefi-
ciary in foam production. As stated previously, carob flour used for
mixture productions was made by grinding the whole carob pod,
together with the seeds. Carob seed endosperm is a known source of
carob bean gum, which is used in food and non-food products as a
thickening and stabilizing agent (Farahnaky et al., 2014). On a molecu-
lar level, the endosperm comprises of galactomanan molecules, which
are hydrophilic biopolymers. They are water soluble polysaccharides
forming highly viscous and stable aqueous solutions (Dos Santos
et al., 2015) and some important properties include holding of H2O,
thickening, gelling, binding, suspending, emulsifying, as well as forma-
tion of films (Srivastava and Kapoor, 2005). In this research, the
BENKOVIĆ ET AL.
galactomannans from the carob seeds acted as foam stabilizers, which
is in accordance with its previously listed properties. Furthermore, it
can be noticed that samples S2 and S4, which contained 20% of carob
flour, 10% cocoa and 70% sugar (with stevia, S4) had the lowest
values of foam stability, indicating that the selection of the appropri-
ate content of carob flour, as well as the carob bean gum concentra-
tion is of great importance.
3.2 | Physical properties
Results for median diameter, Sauter diameter, bulk density and mois-
ture content of mixtures, and foam mat dried powders are shown in
Table 3.
Based on the data shown in Table 3, as the percentage of carob
flour added to the mixture increases, the values of median diameter
decrease, and are the lowest for mixtures S3 and S6 which both con-
tain 30% carob flour. Interestingly, median diameters of the control
mixtures (K1 and K2), containing only cocoa and sugar, exhibited the
highest values of median diameters. This is due to the nature of cocoa
powder: small particles tend to stick to the larger sugar crystals which
act as cores, as previously stated by Benković et al. (2015). Significant
differences (p < .05) and different trends were observed in the case of
Sauter diameter. Sauter diameter of the mixtures increases with the
addition of larger percentage of carob flour to the mixtures, indicating,
if Sauter diameter is observed as particle volume to particle surface
area ratio, a rise in the particle volume and a drop-in surface area of
particles present in the mixture, which was expected, due to larger
particle sizes of the carob flour. The lowest Sauter diameters were
recorded for control samples K1 and K2. Furthermore, the addition of
0.3% of Stevia lead to a slight decrease in both median and Sauter
diameter of these mixtures (S4, S5, S6, and K1) in comparison to
equivalent mixtures without Stevia (S1, S2, S3, and K2). Namely, ste-
via powder had median particle size of <100 μm, which meant that
the amount of low diameter particles in the mixtures was increasing
further with the addition of stevia. The result of a larger portion of
smaller particles in the mixture was a shift of median and Sauter
diameters toward smaller values in comparison to the mixtures
without stevia.
Prior to drying, bulk densities, loose and tapped, exhibited the
same trend: the addition of carob flour lead to an increase of bulk
density values, with samples S3 and S6, exhibiting the highest bulk
density values. On the other hand, samples containing only cocoa and
sugar (K1 and K2) showed the lowest loose and tapped bulk density
values. The same trend was also observed for moisture content: larger
percentages of carob flour in the mixtures lead to higher moisture
content values.
After foam mat drying, median diameter for the majority of the
samples, was lower than prior to drying. Based on the description of
the drying process, when proteins, maltodextrin, and carboxymethyl-
cellulose were dry mixed with the powders, water was added to
obtain a smooth mixture which was then blended. The water addition
dissolved the sugar crystals, which previously represented a high per-
centage of mixture constituents of large particle sizes. In this case,
larger particles were dissolved, due to which smaller median diameters
were obtained for the foam mat dried powders. Furthermore, it can
BENKOVIĆ ET AL. 5 of 11

TABLE 3 Median diameter (d [0.5]), Sauter diameter (D[3,2]), loose (ρ10), and tapped (ρ100) bulk density and moisture content of powder mixtures
and foam mat dried powders
Sample d (0.5) (μm) D [3,2] (μm) ρ10 (kg/m3) ρ100 (kg/m3) Moisture content (%)
Mixtures
S1 486.55  6.70* 37.59  9.351,2,3,6 822.87  19.652,3,5,6,K1,K2 957.96  4.382,3,5,6,K1,K2 1.58  0.052,3,5,6,K1,K2
S2 473.35  12.14 2,6
52.38  1.39 1,3,4,5,6,K1,K2
904.63  14.36 1,3,6,K1,K2
1,018.43  8.30 1,K1,K2
1.90  0.101,3,4,6,K1,K2
S3 434.99  7.04* 87.18  4.46 1,2,4,5,K1,K2
951.42  8.21 1,2,4,K1,K2
1,028.51  21.21 1,4,K1,K2
2.43  0.091,2,4,5,K1,K2
S4 462.35  9.75* 31.58  1.862,3,5,6,K1 844.32  37.523,6,K1 952.90  44.123,6,K1 1.55  0.122,3,5,6,K1
S5 434.67  8.72* 46.09  0.48 2,3,4,6,K1,K2
910.28  9.15 1,6,K1,K2
1,023.14  20.65 1,6,K1,K2
1.97  0.061,3,4,6,K1,K2
S6 428.80  9.95 2,6
80.35  3.00 1,2,4,5,K1,K2
972.07  23.16 1,2,4,5,K1,K2
1,049.39  7.75 1,4,5,K1,K2
2.39  0.031,2,4,5,K1,K2
Control samples
K1 513.77  20.43* 27.94  2.392,3,4,5,6 739.81  22.101,2,3,4,5,6 859.48  11.351,2,3,4,5,6 1.20  0.021,2,3,4,5,6
K2 501.69  4.96* 26.49 3.18 2,3,5,6
749.85  33.21 1,2,3,5,6
852.29  32.35 1,2,3,5,6
1.22  0.091,2,3,5,6
Foam mat dried powders
S1 425.41  0.833,4,K1 151.45  0.596 801.86  20.22K1 867.03  12.122,K1 5.12  0.042,4,5,6,K1
S2 465.00  9.92* 174.91  4.57* 795.09  30.95K1 821.92  4.671,K1 4.79  0.101,3,4,5,6,K1
S3 392.13  7.42 1,4
151.43  1.91 6
793.05  50.42 5,K1,K2
847.12  5.64 5,K2
5.18  0.012,4,5,6,K1
S4 391.67  18.93 1,3,6,K1
190.03  2.61 K1
827.40  66.76* 855.11  6.80 K1
4.57  0.041,2,3,5,6,K1
S5 465.34  7.56* 214.23  4.10* 755.69  36.93 3,6,K1,K2
822.86  4.19 3,6,K1,K2
6.56  0.071,2,3,4,K1
S6 409.61  13.144 174.35  8.471,3,K1 819.29  24.975,K1,K2 864.62  6.015,K2 6.51  0.061,2,3,4,K1,K1
Control samples
K1 386.28  10.591,4 137.27  6.254,6 903.77  20.941,2,3,5,6 955.84  0.001,2,4,5 6.33  0.041,2,3,4,5,6
K2 409.02  5.09* 145.20  3.72* 896.64  47.11 3,5,6
946.81  8.17 3,5,6
5.62  0.65*

*No significant difference at p < .05. 1,2,3,4,5,6,K1,K2

– significant differences (p < .05) among samples with a corresponding number. Results are expressed
as mean  SD.

also be argued that, as no visible trend of the median diameter change
was observed with carob flour addition, median diameter of all the
foam mat dried powders is foremost a result of the subsequent grind-
ing process. Sauter diameter, although higher for all the foam mat
dried powders, also did not show any visible trend of changes with
the addition of carob flour, indicating a dependence on the grinding
process. It must be emphasized that, by implementation of foam mat
drying, food powders with uniform particle size distribution were
obtained in comparison to primary mixtures, which is favorable for
powder handling (graphs shown in the Supporting Information of the
manuscript). In the particle size distribution graphs, Supporting Infor-
mation Figure S1A) shows the particle size distribution of primary mix-
tures, where the first peak (at approximately 10 μm) represents the
cocoa particles. The other peak (approximately 80 to 200 μm) is con-
nected to carob flour and stevia powder and the last peak with sugar
particles. According to literature data, the existence of a wide range of
particle sizes, as well as wide particle size distributions causes flow
problem and unwanted segregation (Barbosa-Canovas et al., 2005). In
the case of the foam mat dried powders (Supporting Information
Figure S1B), the particle size distribution has only one peak (unimodal)
where flow difficulties and segregation can be excluded.
Loose and tapped bulk density of foam mat dried powders is
lower for all the samples (S1 to S6) in comparison to the non-dried
obtained after drying were not as porous and had higher bulk density.
Poor stability during drying is closely connected to density and stabil-
ity of the foams (data shown in Table 2). Foams with higher stability
before the drying experiment began also remained more stable during
drying. As stated previously, mixtures containing the highest percent-
age of carob flour had lower foam density and higher foam stability
due to the presence of galactomanans, and therefore, the foam struc-
ture remained stable during drying. Namely, the carob flour used in
this research was made by grinding whole carob pods containing
carob seeds. Carob seeds are known to contain galactomannans,
which are used as thickeners/stabilizers, co-gellants and fat replacers
in ice creams, sauces and other food products (Pollard et al., 2007). In
this case, the presence of galactomanans lead to foam stabilization
during drying. Furthermore, it is a well-established fact that the addi-
tion of proteins favors the foam production process. In this case, whey
and soy proteins were used as a commercially available preparation
and the same amount of the protein mix was added to all samples. In
this way, the influence of proteins on the final stability of the foams,
their behavior during drying and on the quality of the final product
remained a constant for all samples. Beneficial influences of whey pro-
teins on foam stability appear because of their ability to unfold and
absorb at the interface between the dispersed and the continuous

mixtures. Lower bulk density values are an indication of higher poros- phase and to form a viscoelastic adsorbed layer (Borcherding, Loren-

ity of the foam mat dried powders. An exception was presented in the
form of control samples K1 and K2. In these cases, the foam, although
produced in the same manner as for samples S1 to S6, showed poor
stability during drying, as a result of low foam stability and separation
of the liquids from the foam which was the reason why the powders
zen, Hoffmann, & Schrader, 2008, Wilde, 2000). On the other hand,
soy proteins also have foaming, emulsification and gelling abilities but
these abilities are highly dependent on the type of soy protein (native
or isolate) and extrinsic factors (pH, temperature, ionic strength)
(Shao, Lin, & Kao, 2016).
6 of 11
FIGURE 1 Cohesion index and mean cake strength of the powder
mixtures (before drying) and foam mat dried powders (after drying).
Results are expressed as mean  SD
Moisture content of the mixtures and the foam mat dried pow-
ders is also shown in Table 3. The moisture content of the mixtures
was dependent on the composition of the mixtures and the content
of carob flour. Mixtures with higher percentage of carob flour also
exhibited the highest moisture content (S3 and S6). The mixtures
without the addition of carob flour (K1 and K2) exhibited the lowest
moisture content. This was due to the higher initial moisture content
of the carob flour as a raw material in comparison to sugar and cocoa
powder. Moisture content values of all the foam mat dried powders
indicated they were all successfully dried to a desired moisture con-
tent in the range approximately 4.5 to 6.5%. Differences in moisture
content among foam mat dried samples cannot be attributed to the
difference in carob flour content, as no clear pattern in moisture con-
tent change was detected.
Flow properties of mixtures and the foam mat dried powders were
assessed by a powder rheometer test, determining the powders cohesiv-
ity and the susceptibility to caking. Results of are shown in Figure 1.
Cohesion index values before and after drying is shown in
Figure 1a. Powder mixtures prior to drying had higher cohesion index
values. An exception was noticed for sample S3, which had a slightly
higher cohesion index after drying, but this difference is small and can
be attributed to inherent statistical positioning of the particles in a
measuring vessel. According to literature data, powders with cohesion
indices higher than 19 are considered to be extremely cohesive, from
16–19 very cohesive, from 14–16 cohesive, 11–14 easy flowing
and < 11 free flowing (Shah et al., 2008). Based on this categorization
scale, mixtures S1 and K2 were considered extremely cohesive,
BENKOVIĆ ET AL.
mixtures S2, S4, S5, and K1 were classified as cohesive or very cohe-
sive, while the mixtures S3 and S6 with the highest percentage of
carob flour were in the free flowing range, even before drying. This
was an indication that, once again, cohesiveness of the mixtures was
dependent on the amount of carob flour added to the mixtures. Mix-
tures containing more carob flour also had higher values of D[3,2]
(Table 3) and based on literature data, powders with larger particle
sizes are less susceptible to cohesion (Barbosa-Canovas et al., 2005).
For foam mat dried powders, cohesion index values were considerably
lower than for powder mixtures which were not dried. The foam mat
dried powders can be classified as free or easy flowing in all cases.
Small differences among cohesion index values were an indication
that, in this case, cohesion index was not dependent of the composi-
tion of the mixture, but on the milling process. Foam mat drying pro-
cess resulted in powders with higher Sauter diameter, which lead to
the lower cohesivity of these powders. On the other hand, as argued
before, the foam mat dried powders’ particle size distribution has only
one peak (unimodal) where flow difficulties and segregation can be
excluded. These results indicate that the foam mat drying process
resulted in free-flowing powders with markedly lower cohesion
indexes, which is a favorable property while handling and processing
powders in an industrial environment.
Mean cake strength, as a mean of evaluation of proneness to caking,
is shown in Figure 1b. Similar to cohesion index, mean cake strength
values are also considerably lower for foam mat dried powders. The dif-
ference in mean cake strength is especially notable for samples control
samples K1 and K2, with no addition of carob flour. In these cases, parti-
cle size enlargement from small cocoa powder particles to foam mat
dried powders acted as an improver of flow properties.
When improving powder properties by drying, reconstitution
properties have to also be taken into account, making the powder eas-
ily dissolvable and dispersed. Solubility and dispersibility data is shown
in Figure 2.
Based on dispersibility data shown in Figure 2a, it can be
observed that higher percentage of carob flour added to the mixtures
prior to drying caused a drop-in time taken to disperse the samples.
The difference between mixtures with (S1 to S6) and without carob
flour (K1 and K2) is especially pronounced, as cocoa powder contains
10–12% fat, which aids lump formation. Namely, cocoa powder is
known for high fat content which is then reduced to 10–18% during
production, while carob flour, according to literature data, contains
only 0.8–2.5% fat (Durazzo et al., 2014). After drying, dispersibility
was markedly improved for mixtures which contained larger amounts
of cocoa powder (S1, S2, S4, and S5), and the opposite trend was
observed for mixtures which contained only carob flour (S3 and S6).
In this case, formation of porous particles and subsequent grinding did
not improve dispersibility, probably due to higher galactomannan con-
tent from carob seeds present in the samples. According to a study by
 ski, and Orczykowska (2017), galactommanans were
Jóźwiak, Dziubin
characterized as substances with poor reconstitution properties due
to low hydrophobization of their surfaces.
Solubility of the samples was improved for samples S1, S3, S6,
K1, and K2. It is important to emphasize that the solubility method
used in this study relies on the amount of insoluble material left in the
BENKOVIĆ ET AL. 7 of 11

TABLE 4 Total polyphenol content (gallic acid equivalents) and

antioxidative capacity (Trolox equivalents) of powder mixtures and
foam mat dried powders. Results are expressed as mean  SD
Total polyphenolic content Antioxidative capacity
Sample (mg GAE/g sample) (mg TE/g sample)
Powder mixtures
S1 7.14  0.072,3,5,6,K1,K2 8.51  0.99all
S2 4.94  0.31 1,3,6,K1,K2
6.29  0.22all
S3 1.46  0.17 1,2,4,5,K1,K2
1.79  0.361,2,4,5,K1,K2
S4 6.48  1.053,5,6,K1,K2 7.24  0.46all
S5 4.63  0.12 1,3,4,6,K1,K2
5.33  0.14all
S6 1.72  0.07 1,2,4,5,K1,K2
2.27  0.131,2,4,5,K1,K2
Control samples
K1 11.51  1.151,2,3,4,5,6 11.93  0.501,2,3,4,5,6
K2 12.14  1.11 1,2,3,4,5,6
12.78  0.271,2,3,4,5,6
Foam mat dried powders
S1 3.53  0.02all 3.43  0.263,5,6,K1,K2
S2 2.53  0.221,3,6,K1,K2 3.03  0.283,6,K1,K2
S3 1.04  0.02 1,2,4,5,K1,K2
0.73  0.01all
S4 2.96  0.04 1,3,5,6,K1,K2
3.13  0.133,5,6,K1,K2
S5 2.05  0.10 1,3,4,6,K1,K2
2.35  0.131,3,4,6,K1,K2
S6 1.08  0.061,2,4,5,K1,K2 1.07  0.04all
Control samples
K1 4.47  0.321,2,3,4,5,6 5.03  0.16 all

FIGURE 2 Dispersibility (a) and solubility (b) of powder mixtures prior K2 4.49  0.18 1,2,3,4,5,6
6.31  0.13 all
to drying and the foam mat dried powders. Results are expressed as all
Significant differences detected among all samples at p < 0.05.
mean  SD – significant differences (p < 0.05) among samples with a
1,2,3,4,5,6,K1,K2

corresponding number.
graded cuvette after centrifugation, which is not as precise for
samples with similar solubility. A more precise approach would be to 2010, Rimbach et al., 2009). On the other hand, biological effects of

modify this method so the insoluble material is dried and weighed carob flour associated with the high contents of polyphenols, have

after separation. also been documented (Avallone et al., 2002, Vitali Čepo et al., 2014).

Furthermore, the results obtained for both dispersibility and Based on the total polyphenol content data for powder mixtures

solubility also depend on the drying process. Literature data states shown in Table 4, control samples (K1 and K2), containing only cocoa

that the type of the drying process, temperature and the type of powder had the highest levels of polyphenols. As the amount of carob

proteins and gums used affects the porosity and, therefore, the flour in the mixtures increased, the level of total polyphenols started

final result of the drying process (Sundaram and Durance, 2007, decreasing, indicating that cocoa powder was a predominant source

Begum et al., 2017). In this study, on one hand, drying could have of polyphenols. Furthermore, this was also a clear indication that, to

caused a change in protein conformation, as reported by Katekhong obtain high polyphenol content, only a small part of cocoa powder can

and Charoenerin (2017), which subsequently affected porosity and be replaced by carob flour, up to 10% (samples S1 and S4). For foam

reconstitution properties. On the other hand, the presence of mat dried powders, the detected amount of polyphenol compounds

galactommanans and their structural changes during drying could was lower in comparison to powder mixtures before drying, indicating

have affected the reconstitutution properties. However, to offer a a degradation of heat sensitive bioactive compounds. Furthermore,

more plausible explanation in changes in molecular structures, due to poor stability of some foams (e.g., K1 and K2) and the separa-

further research is needed.
3.3 | Total polyphenol content and antioxidant
capacity
Total polyphenol content and antioxidant capacity were monitored to
get an insight on the influence of drying and increased carob flour
content on the bioactive profile of the mixtures, as well as on the
foam mat dried powders. Results are shown in Table 4.
Cocoa powder is a natural rich source of antioxidants, which
include polyphenols, mainly flavonoids (Abbe Maleyki and Ismail,
tion of the liquid phase during drying, the drying time was prolonged
to 24 hrs and, to make the samples intercomparable, it was decided to
dry all of them for 24 hrs (even the more stable ones). Visual inspec-
tion of unstable foams even after several hours of drying (e.g., K1 or
K2) revealed they were not dry enough and that such foam could not
be milled into a powder and thus the longer drying process. Longer
duration of the drying process (24 hr) required to obtain a mat dry
enough to be suitable for milling in this case led to bioactive com-
pounds degradation. The losses in total polyphenols content were
especially notable for the K1 and K2 mixtures which contained only
cocoa powder (e.g., for K2 total polyphenolic content dropped from
8 of 11
FIGURE 3 Radar diagrams of sensory analysis of the powder mixtures before drying (a) and foam mat dried powders (b)
12.29 to 4.76 mg GAE/g d.w., which leaves only 38.73% of the poly-
phenols present in the initial non-dried mixture). However, the drop-
in polyphenols content was not as distinguished for mixtures with
higher carob flour content. For example, mixture S3 contained
1.10 mg GAE/g d.w. of total polyphenols after drying, which is as high
as 73.82% of the initial value before drying. This was an indication
that the presence of carob flour in the mixtures benefits the preserva-
tion of total polyphenols during the foam mat drying process. Better
preservation of total polyphenols of carob flour containing samples
can be attributed to two factors. First, carob polyphenols are cova-
lently bound to dietary fibers (Goulas et al., 2016), which do not show
a decrease in concentration during processing, but only a change in
soluble and insoluble fraction (Kutoš et al., 2003). They could have
acted as polyphenol protectors in this case. On the other hand, dietary
fiber can also have antioxidant properties (Elleuch et al., 2011). The
second explanation is connected to the sole nature of the carob fruit.
Namely, the carob fruit grows in Mediterranean regions, known for
BENKOVIĆ ET AL.
high temperatures and low rainfall during the period of carob
growth and harvesting. To adapt to the harsh environmental condi-
tions, the carob fruit cells have developed wide and hardened cell
walls which act as barriers for heat and mass transfer (Benković
et al., 2016), which is also beneficial for bioactive compounds
preservation.
The highest antioxidant capacity before drying was determined
for samples K1 and K2 and the lowest for samples S3 and S6, which
only contained carob flour and sugar (Table 4). In this case, it was also
clear that only a small amount of cocoa powder (10%) can be replaced
by carob flour to get powders with high antioxidant capacity. After
drying, initial values of antioxidant capacity dropped to approximately
40 to 52% of the initial value. The highest drop in antioxidant capacity
was detected for sample K2 (51.62%), and the lowest for sample S1
(41.73%). It this case, the preservation of antioxidant capacity after
drying was not dependent on the amount of carob powder added to
the mixtures.
BENKOVIĆ ET AL.
FIGURE 4 Principal component analysis of physical, chemical and
sensory properties of powder mixtures (a) and foam mat dried
powders (b). The letter “P” in front of the sensory attribute refers to
“powder” and the letter “D” for the prepared drink. “TPC” stands for
total polyphenolic content, “ABTS” for antioxidant capacity
determined by the ABTS method, “ro” for bulk density at a specified
number of taps, CI for cohesion index and MCS for mean cake
strength
3.4 | Sensory properties
Prior to drying, samples containing only carob flour (S3, S6) received
the lowest grades ones on every grading point for powder, as well as
for the drink (Figure 3a). This was an indication that consumers did not
prefer total elimination of cocoa powder from such products. The high-
est scores were obtained for sample S4, which contained 10% of carob
flour, 20% cocoa powder, 69.7% sucrose, and 0.3% of stevia. This is a
confirmation of the previously discussed results for chemical proper-
ties: to contain good chemical and sensory properties only a small part
of cocoa powder can be replaced by carob.
In direct comparison of the grades before (Figure 3a) and after
drying (Figure 3b), it was visible that the scores for drink sweetness
and aftertaste for prepared foam mat powder drinks were slightly
lower than for the drinks prepared with original mixtures. For mixtures
containing larger amount of cocoa powder, sweetness of foam mat
dried powders was markedly lower, which also lead to lower grades
for aftertaste. Foam mat powders with larger amount of carob flour
received better scores for sweetness and aftertaste after drying,
which was an indication that carbohydrates present in carob flour
contribute to taste preservation during the foam mat drying process.
9 of 11
Furthermore, it is important to emphasize that foam mat dried pow-
ders received better scores for powder odor, color and appearance. In
general, the sensory analysis indicated that sample S4 (10% carob +
20% cocoa + 69.7% g sucrose + 0.3% stevia) was the most acceptable
for consumers.
3.5 | Principal component analysis and correlations
between physical, chemical, and sensory properties
Principal components and classification analysis was performed using
the experimental data for physical, chemical, and sensory properties
of the mixtures and dried powders. Results are shown in Figure 4.
The first two components accounted for 92.16% of the variability
in the results for powder mixtures before drying and for 71.97% of
the variability for foam mat dried powders. Mixtures S2, S5, S3, and
S6 before drying (Figure 4a) were clearly separated based on their
physical properties (bulk density at 10 and 100 taps, moisture content,
particle size, and solubility). Total polyphenols, ABTS, mean cake
strength (MCS), cohesion index (CI), and dispersibility were situated in
the second quadrant, as well as the samples K1 and K2, indicating that
these two samples were distinctive from the other based on their high
total polyphenolic content, antioxidant capacity and differences in
flow properties (CI and MCS). Sensory attributes were situated in the
third quadrant in which samples S1 and S4 are grouped, which were
considered to have the most acceptable sensory properties.
After drying, the variability between the samples was not
explained as successfully as before drying, as the first two factors
explained only 71.97% of the total variance (Figure 4b), in comparison
to 92.16% explained for the mixtures before drying. Sensory attri-
butes are all situated in the first quadrant, together with samples S1
and S4, which received the highest sensory scores. Samples S2 and S5
are distinctive based on their particle size, MCS and solubility (situated
in the second quadrant) and samples S3 and S6 based on moisture
content (third quadrant). Samples K1 and K2 are situated in the fourth
quadrant, differing from the others based on TPC, antioxidant capac-
ity, bulk density, dispersibility, and cohesion index.
In this research, PCA analysis successfully separated physical,
chemical, and sensory properties of both mixtures and the foam mat
dries powders. Samples which were different or exceptional in compari-
son to others based on a certain property were confirmed as such based
on PCA analysis (e.g., samples K1 and K2 with high TPC and antioxidant
capacity values were oriented along the stated properties in the factor
plane. Furthermore, the PCA also indicated and confirmed similarities
among samples. For example, mixtures S3 and S6, in which the whole
amount of cocoa powder was replaced by carob stood out based on
their solubility prior to drying and moisture content after drying. Based
on these observations, PCA analysis proved to be a useful tool in distin-
guishing the differences as well as similarities among samples.
4 | CONC LU SIONS
The aim of this article was to determine the effect of substitution of
cocoa powder with carob and sucrose with stevia on physical, chemi-
cal, and sensory properties of powdered drink mixes and to assess the
10 of 11
adequacy of foam mat drying for production of cocoa/carob instant
powders.
Addition of carob flour to cocoa powder mixtures improved phys-
ical properties of the mixtures. Foam mat drying further lowered the
cohesion index and mean cake strength, which is favorable for powder
handling. Analysis of chemical properties showed that high values of
total polyphenols and antioxidant capacity can be maintained only if a
small portion (10%) of cocoa powder is replaced by carob flour. Foam
mat drying led to loss of total polyphenols, which was more pro-
nounced for powders which had higher percentages of cocoa powder.
Overall, to obtain a foam mat dried powdered product with good
physical, chemical, and sensory characteristics, only a small part of
cocoa powder can be replaced by carob flour (up to 10%).
ACKNOWLEDGMENT
The research is funded by Croatian Science Foundation. Grant num-
ber: IP-11-2013-3304-TEUCLIC.
CONF LICT OF IN TE RE ST
The Authors declare no conflict of interest.
ORCID
Maja Benković http://orcid.org/0000-0003-2167-6862
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SUPPOR TI NG I NFORMATION
Additional supporting information may be found online in the Sup-
porting Information section at the end of the article.
How to cite this article: Benković M, Radić K, Vitali Čepo D,
et al. Production of cocoa and carob-based drink powders by
foam mat drying. J Food Process Eng. 2018;41:e12825. https://
doi.org/10.1111/jfpe.12825