processes

Article
Mathematical Modeling and Optimization of Ultrasonic
Pre-Treatment for Drying of Pumpkin (Cucurbita moschata)
Sven Karlović , Filip Dujmić , Suzana Rimac Brnčić *, Marija Badanjak Sabolović,
Antonela Ninčević Grassino , Marko Škegro , Marko Adrian Šimić and Mladen Brnčić

Faculty of Food Technology and Biotechnology, University of Zagreb, 10000 Zagreb, Croatia
* Correspondence: [email protected]

Abstract: Innovations in food drying processes are usually aimed at reducing drying time and
improving the overall properties of dried products. These are important issues from an economic
and environmental point of view and can contribute to the sustainability of the whole process. In this
study, the effects of ultrasonic treatment on the drying kinetics of pumpkin pulp are investigated, and
mathematical models to predict the drying kinetics are analyzed and optimized. The results show
that ultrasonic pretreatment significantly reduces drying time from 451 to 268 min, with optimal
processing parameters at 90% of the maximum ultrasonic power and a processing time of 45 min.
The total color change of the samples was the lowest at the obtained optimal processing parameters.
Based on the values (RMSE and R2 ) of the investigated mathematical drying models, it was found that
the Weibull model is the best fit for the experimental data and is considered suitable for the drying
kinetics of ultrasonically pretreated pumpkin samples. In this study, an artificial neural network
with 15 neurons in hidden layers was also used to model the drying process in combination with
ultrasound pretreatment. The network had a performance of 0.999987 and the mean square error was
8.03 × 10−5 , showing how artificial neural networks can successfully predict the effects of all tested
process variables on the drying time/moisture ratio.

Keywords: pumpkin; drying; ultrasonics; mathematical models

Citation: Karlović, S.; Dujmić, F.;
Brnčić, S.R.; Sabolović, M.B.;
Ninčević Grassino, A.; Škegro, M.;
Šimić, M.A.; Brnčić, M. Mathematical
1. Introduction
Modeling and Optimization of
Ultrasonic Pre-Treatment for Drying The pumpkin belongs to the wide family of cucurbits (Cucurbitaceae), and the three
of Pumpkin (Cucurbita moschata). most common varieties of pumpkin are called Cucurbita maxima, Cucurbita moschata, and
Processes 2023, 11, 469. https:// Cucurbita pepo [1,2]. Europe is the second-largest producer with approximately 4.9 million
doi.org/10.3390/pr11020469 tons of pumpkin, which is about 17.5% of world production [3]. However, since pumpkin is
mainly used for seeds, decorative purposes, and as animal feed, large amounts of waste and
Academic Editor: Dariusz Dziki
by-products are generated during industrial processing. In general, seeds represent 10%
Received: 16 December 2022 of the total weight, whereas about 90% of pulp and peel are discarded, having previously
Revised: 20 January 2023 been considered as waste [4]. The pulp and peel contain many functional compounds such
Accepted: 30 January 2023 as polyphenols, carotenoids (mainly β-carotene), vitamin C, low-energy sugars, and a large
Published: 3 February 2023 amount of dietary fiber [5]. Pumpkin, as a cultivar that is widespread throughout the world,
is recognized as one of the three medicinal plants beneficial for diabetes [6]. The chemical
and biochemical composition of pumpkin has been extensively researched and it has
been proven that pumpkin is a rich source of vitamins and minerals [7], essential nutrients,
Copyright: © 2023 by the authors.
phenols, flavonoids, and carotenoids [8], and antioxidants [9]. Thus, pumpkin has beneficial
Licensee MDPI, Basel, Switzerland.
effects on human health [8], reduces the risk of neurodegenerative, cardiovascular, and
This article is an open access article
distributed under the terms and
cancer diseases [10] and prevents osteoporosis and hypertension [11,12].
conditions of the Creative Commons
Drying is the most commonly used method for food preservation and extending its
Attribution (CC BY) license (https:// shelf life [13,14]. Due to rising energy prices, food drying is an energy-intensive process
creativecommons.org/licenses/by/ that consumes up to 15% of energy in all food industries combined [15]. There is a growing
4.0/). interest in the use of ultrasound in co- or pre-processing for drying. The use of ultrasound

Processes 2023, 11, 469. https://doi.org/10.3390/pr11020469 https://www.mdpi.com/journal/processes

 Drying is the most commonly used method for food preservation and extending its
shelf life [13,14]. Due to rising energy prices, food drying is an energy-intensive process
Processes 2023, 11, 469 that consumes up to 15% of energy in all food industries combined [15]. There is a growing 2 of 13

interest in the use of ultrasound in co- or pre-processing for drying. The use of ultrasound
in the treatment of food raw materials, wastes and by-products shows promising results
forthe
in versatile
treatment applications,
of food raw both in primary
materials, research
wastes and in industry
and by-products shows[16–20].
promising results
In general,
for versatile sonication/ultrasound
applications, both in primary represents
researchaandsound that is inaudible
in industry [16–20]. to humans be-
cause In the
general, sonication/ultrasound
ultrasound frequency startsrepresents
at 18 kHz,a which
sound that is inaudible
is inaudible to humans
to humans. be-
Ultra-
cause
soundthe ultrasound
with such power frequency
is usedstarts at 18variety
in a wide kHz, which is inaudiblesuch
of applications, to humans. Ultrasound
as extraction, emul-
with such power
sification, is used in a sieving,
homogenization, wide variety of applications,
sedimentation, such as extraction,
micronization, emulsification,
pasteurization, cell dis-
homogenization, sieving, sedimentation, micronization, pasteurization,
ruption, drug delivery, sterilization, wastewater treatment, and in general food pro- cell disruption,
drug
cessingdelivery,
[21–24].sterilization, wastewater treatment, and in general food processing [21–24].
Low-frequency
Low-frequencyultrasound
ultrasound(18–100(18–100 kHz),
kHz),with low
with to high
low intensities,
to high expressed
intensities, by the
expressed by
diameter of the −2 is most commonly used for treatments. Among
the diameter of probe
the probe(5–1000 W/cm
(5–1000 W/cm),−2), is most commonly used for treatments. Among
these
theseultrasound
ultrasoundparameters,
parameters,thethe propagation
propagation of sound
of soundwaves showed
waves greatgreat
showed potential [25].
potential
When the research aims at the gentle propagation of ultrasound
[25]. When the research aims at the gentle propagation of ultrasound waves considering waves considering the
applied
the applied intensities, ultrasound baths (indirect treatment) are used as devices, whilethe
intensities, ultrasound baths (indirect treatment) are used as devices, while on on
other hand,
the other when
hand, whenhigh intensities
high intensitiesareare
required,
required,devices
devices with
withdirectly
directlyimmersed
immersedprobes
probes
(direct
(directtreatments)
treatments)are areused
used[26].
[26].
Figure
Figure 1 shows the mostcommon
1 shows the most commonultrasonic
ultrasonicdevices
devicesusedusedfor
forfood
foodprocessing.
processing.

Figure 1.1. Most

Figure Most common
common ultrasonic
ultrasonicsetups:
setups:(A)
(A)bath
bathwith probes
with mounted
probes bellow:
mounted (B) (B)
bellow: directly im-
directly
mersed probe: (C) continuous flow sonication with cooling.
immersed probe: (C) continuous flow sonication with cooling.

Eachof
Each ofthe
thepresented
presentedultrasound
ultrasounddevices
devicesisisequipped
equippedwithwiththe
thefollowing
followingfourfourbasic
basic
elements:An
elements: an ultrasound
ultrasoundgenerator,
generator,an anultrasound
ultrasoundtransducer,
transducer, a probe
a probe or or probes
probes depend-
depending
ingthe
on onsystem
the systemand aand a treatment
treatment chamber
chamber as The
as well. well.main
The mechanism
main mechanism of ultrasonic
of ultrasonic work
work
in in the medium
the liquid liquid medium
is basedison based on the generation
the generation and implosion
and implosion of gas cavitation
of gas cavitation bubbles
bubbles
in in theliquid
the treated treated liquid medium.
medium. CavitationCavitation
bubbles bubbles are created
are created in the vicinity
in the vicinity of the
of the liquid
liquid treated
treated by the by the ultrasonic
ultrasonic waves,waves,
whichwhich are subjected
are subjected to rapid
to rapid and alternating
and alternating pres-
pressure
with
sure high
with amplitude.
high amplitude.In theInphysics of sound,
the physics therethere
of sound, are negative and and
are negative positive pressure
positive pres-
cycles, i.e., during
sure cycles, the negative
i.e., during half of this
the negative halfphenomenon, the treated
of this phenomenon, sample
the is stretched,
treated sample is
while
stretched, while in the positive half it is compressed. The resulting microbubbles during
in the positive half it is compressed. The resulting microbubbles vary in size vary in
the
sizenegative
during the andnegative
positive and
pressure cycles
positive until the
pressure finaluntil
cycles phenomenon, implosion, occurs.
the final phenomenon, implo-
sion,When
occurs. the bubbles implode, they release enormous amounts of energy in the form of
high pressure (up to 100 MPa) and high temperatures (up to 5000 K) [27]. However, the
release of all the accumulated energy results in local pressure and temperature changes
that dissipate in the liquid in the chamber. This local energy propagates into the liquid
environment and causes structural, chemical, and physical changes in the immersed sam-
ple [28]. In addition, ultrasound has the advantage of non-thermal technology and thus
has a positive impact on the environment.
Processes 2023, 11, 469 3 of 13

Ultrasound as a pretreatment in food drying is gaining increasing attention, as it does

not only shorten the drying time, but also helps to reduce energy consumption [29,30].
The mechanical and thermal effects of ultrasonic cavitation can shorten drying time by
altering or destroying the cellular matrix. It can also contribute to the removal of the wax
coating [31]. Both effects lead to an improvement in the mass and heat transfer with each
further drying process (vacuum, microwave, conventional, etc.) [32–34]. The drying process
usually has two or three periods. The first is a period in which the drying rate is constant
(so that the drying curve is practically linear), followed by a period of decreasing drying
rate. During the second period, the water evaporates from the surface of the material, while
the water inside the material diffuses to the surface through the pores of the cell matrix.
Ultrasonic treatment increases the size and number of pores, thus accelerating mass transfer
and shortening the drying time. Mathematical models have been used to describe the
kinetics of mass transfer in convective drying processes as a function of drying conditions,
such as temperature or pressure. Modeling the drying process can help improve drying
efficiency, shorten drying time, and thus improve time and energy efficiency as well as the
sustainability of the drying process. Modeling is a much simpler and faster method for
predicting optimal process parameters and conditions to achieve desired outcomes, such as
product quality. It is also a tool to design and size dryers for specific requirements. Many
authors have already analyzed and improved mathematical models for drying various
food products such as apples, kiwi and other fruits [35–37]. Some limitations and problems
with the drying models are that most models are based on a two-step procedure. In the
first step, the best model was calculated based on the dependence between water content
and drying time, and various errors such as R2 or χ2 were obtained for each model. The
second step involves the calculation of model constants and coefficients as a function of
process parameters such as drying temperature, air velocity, etc. This approach leads to
the continuous development of minimally-modified models that excellently describe the
drying curves for a specific drying process. This is due to the obtained coefficients, which
have no physical meaning or relation to physical processes such as mass and heat transfer.
Therefore, such coefficients cannot be correlated with process parameters. Efforts have been
made to create more general empirical mathematical models, with some success. However,
relatively new modeling techniques such as the use of artificial neural networks have much
greater potential to capture a larger number of parameters. Such heuristic models may be
better suited to complex and nonlinear processes such as drying combined with ultrasonic
(pre)treatment.
The main objective of this study is to select and develop mathematical models for
the drying of pumpkin and to optimize the parameters of ultrasonic drying to minimize
the drying time. Based on the results, standard empirical models will be compared to the
obtained artificial neural networks.

2. Materials and Methods

2.1. Plant Materials
Fresh pumpkin fruits (Cucurbita moschata) that were uniform in size and undamaged
were selected in late August (about 110 days after ripening) and purchased at the local
market. Because pumpkins can vary significantly in size and other physical characteristics,
those selected from the obtained batch were measured. The pumpkins were pear-shaped
and elongated, with weights of 2.41 ± 0.35 kg and lengths of 30.72 ± 2.48 cm.
Fruits were transported to the laboratory, washed with tap water, and stored in the
refrigerator at 4 ± 1 ◦ C until further use. Before starting the experiment, the fruits were
removed from the refrigerator and stored at room temperature (23 ± 1 ◦ C) for about 45 min
to acclimate them to room temperature [38,39]. The fruits were then washed, peeled, and
cut in half lengthwise with a stainless-steel knife. The seeds and fibrous strands were then
separated from the pulp. The pulp was cut into uniform pieces 4–5 mm thick and 15 mm
long using a mechanical slicer.
Processes 2023, 11, 469 4 of 13

The initial moisture content of the fresh pumpkin was determined by oven drying
at 105 ◦ C for 24 h using an electric conduction oven (VO200 PM200 Memmert GmbH,
Büchenbach, Germany), as described in AOAC [40]. Three repeated measurements were
performed.

2.2. Ultrasound Pretreatment

The prepared pumpkin samples were immersed in an ultrasonic bath filled with 7 L
of distilled water (Elmasonic P 300 H, Elma–Hans Schmidbauer Gmbh & Co., Singen,
Germany). Sonication was performed at a constant frequency of 37 kHz for amplitudes
at 30, 60, and 90%. The processing times were 30, 45, and 60 min. The container with the
sample was placed in the same position and the water level in the bath tank was kept at
a height of 270 mm [41]. During the treatment, stainless steel meshes were placed on the
samples to reduce movement.

2.3. Drying Experiment

Before drying, the water content of each pumpkin was measured using an infrared
dryer (LJ16, Mettler-Toledo, Leicester, UK). The average water content of the pumpkin pulp
was 92.10 ± 2.18%.
Samples were dried in a VO200 PM200 conduction vacuum dryer (Memmert
GmbH + Co. KG, Schwabach, Germany) at a temperature of 60 ◦ C [42] and atmospheric
pressure of 1000 mBar. The 360 g of samples was divided into two batches and dried on two
stainless-steel shelves (180 g each). Stainless-steel meshes were placed on the samples for
better heat transfer and a larger contact surface. Water loss during drying was measured
every 10 min using a laboratory balance (Mettler Toledo ME1002TE, Columbus, OH, USA).
Drying was carried out until a constant mass was reached.

2.4. Color Measurement

The color of the fresh and dried samples was determined using a colorimeter (Konica
Minolta CM-3500d, Tokyo, Japan). The total color change (∆E) was the parameter used for
the overall color difference evaluation between a dried and a fresh sample. Based on the
referent sample (fresh pumpkin), ∆E was calculated based on the following equation:
r
 2  2  2
∆E = Lre f − L + are f − a + bre f − b

where L indicates lightness, a is the redness, and b is the yellowness; Lref , aref and bref are
values for the referent sample; and L, a and b are values of the investigated samples.

2.5. Mathematical Modeling

Mathematical models were selected from the already established simple and more
complex models used for the prediction of drying kinetics based on the obtained data,
which are presented in Table 1.

Table 1. Mathematical models for convection drying.

Model Equation References

Page MR = exp(−ktn )
Modified Page MR = exp(−(kt)n ))
[35,36]
Weibull MR = exp((−t/α)β )
Modified two-term MR = a*exp(−k*t) + (1 − a)*exp (−k*a*t)
MR—moisture ratio; a, k—coefficients, n—drying exponent.

Two artificial neural networks (ANN) were trained in Statistica software based on
the drying data obtained. As in the modeling, the output variable for both ANNs was the
moisture ratio (MR). The input variable for the first ANN (further labeled as ANN-1) was
Processes 2023, 11, 469 5 of 13

based on the optimal parameters for the process variables based on the statistical analysis.
For the second ANN (labeled as ANN-2), data obtained for all process variables (process
time 30, 45 and 90 min; amplitude 30, 60 and 90%) were used. Two-thirds of the data was
used for training and one-third was used for the validation of the model.

2.6. Data Analysis

All analyses were performed using Statistica 13 software (Tibco Statistica 13.3.0).
Values were compared using mean comparisons, ANOVA analysis, and Tukey HSD post
hoc test to determine significance. The models presented in Table 1 were fitted using
non-linear estimation regression analysis based on the Levenberg–Marquardt method.
Evaluation of fit of the selected thin layer drying models was based on the coefficient of
determination (R2 ) and root mean square error (RMSE). The highest R2 (closer to unity)
value and a low RMSE (closer to zero) value were the primary criteria for the selection of
the best model [37].

3. Results and Discussion

3.1. Modeling
One way to differentiate mathematical models for predicting drying kinetics can be
based on their perceived complexity. Most basic models, such as that of Page of Lewis, use
only one parameter, while more complex models, such as that of Midilli, may have three
or more parameters. This could significantly improve fitting to experimental drying data,
especially for not-so-standard drying curves compared to those usually observed in the
conventional thin-layer drying of fruits and vegetables. In our drying experiments with
ultrasonic pretreatment, curves such as sigmoidal curve I and II were obtained. However,
due to the very large number of models in the literature and the often insignificant differ-
ences in results and errors, it is inefficient and unnecessary to test them all. In order to avoid
random selection of the appropriate models and to reduce the time required for the analysis,
the selection of the models was based on a review of thin-layer drying models [43,44]. For
the purpose of screening and to reduce the number of models presented, the Lewis model
was tested; however, we did not observe an adequate fit to the experimental data obtained
for the ultrasonically processed samples, with the highest R2 = 0.817 (at 30%, 30 min). Some
other commonly used models such as the Wang and Singh, Geometric, and Singh model
were also discarded as these also were not optimal for the drying curves. Therefore, among
the simpler models, only the Page and the modified Page model and among the more
complex models, the modified two-term model and the Weibull model were selected for
modeling.
The calculated coefficients of determination and RMSE values are shown in Tables 1–4.
It is evident that despite having only one coefficient, the goodness of fit for untreated
samples was best for Page’s model with an R2 of 0.9995.
While the Page model still shows a good fit for the ultrasound pretreatment of the
drying process, increasing the ultrasound amplitude leads to a decrease in the coeffi-
cient of determination and an increase in the RMSE. The Weibull model showed the
best fit for ultrasound treatment with a minimal R2 = 0.9906 for 60% of the amplitude
and maximal R2 = 0.9991 at 40% of maximal amplitude, which is consistent with other
research papers [37–39,45]. The modified two-term model with three variables, which was
expected to fit the experimental data best, demonstrated a good enough fit to be used, but
the much simpler Page and modified Page models were better. The goodness of fit of all
the models tested is in direct correlation to the ultrasound amplitude, since an increase
in amplitude leads to a decrease in R2 values. It is also directly related to the duration of
ultrasound treatment, with minimal R2 obtained for samples with a treatment duration of
60 min. All models show a minimal but visible underestimation of the moisture ratio in the
constant rate period and a slight overestimation in the falling rate period, as can be seen in
Figure 2 for untreated and treated samples.
Processes 2023, 11, 469 6 of 13

Table 2. Coefficient of determination and RMSE of selected mathematical models—30 min treatment.

Model US Power/% R2 RMSE

0 0.9995 0.0010
30 0.9623 0.0056
Page
60 0.9784 0.0051
90 0.9442 0.0078
0 0.9990 0.0015
30 0.9624 0.0062
Modified Page
60 0.9790 0.0060
90 0.9457 0.0083
0 0.9990 0.0006
30 0.9917 0.0011
Weibull
60 0.9974 0.0020
90 0.9940 0.0019
0 0.9997 0.0018
30 0.9602 0.0035
Modified two-term
60 0.9762 0.0029
90 0.9418 0.0054

Table 3. Coefficient of determination and RMSE of selected mathematical models—45 min treatment.

Model US Power/% R2 RMSE

30 0.9981 0.0018
Page 60 0.9675 0.0044
90 0.9334 0.0178
30 0.9957 0.0014
Modified Page 60 0.9652 0.0033
90 0.9314 0.0081
30 0.9991 0.0015
Weibull 60 0.9933 0.0025
90 0.9978 0.0042
30 0.9929 0.0030
Modified two-term 60 0.9635 0.0187
90 0.9373 0.0231

Table 4. Coefficient of determination and RMSE of selected mathematical models—60 min treatment.

Model US Power/% R2 RMSE

30 0.9801 0.0029
Page 60 0.9860 0.0043
90 0.9421 0.0082
30 0.9759 0.0033
Modified Page 60 0.9814 0.0027
90 0.9373 0.0195
30 0.9952 0.0019
Weibull 60 0.9906 0.0014
90 0.9968 0.0034
30 0.9747 0.0034
Modified two-term 60 0.9816 0.0027
90 0.9288 0.0109
 tested is in direct correlation to the ultrasound amplitude, since an increase in ampli
leads to a decrease in R2 values. It is also directly related to the duration of ultraso
treatment, with minimal R2 obtained for samples with a treatment duration of 60 min
models show a minimal but visible underestimation of the moisture ratio in the con
Processes 2023, 11, 469 7 ofseen
rate period and a slight overestimation in the falling rate period, as can be 13 in Fi
2 for untreated and treated samples.

Figure2. 2.
Figure Relationship
Relationship between
between the moisture
the moisture ratio and ratio
dryingand
timedrying
withouttime without
US and US and
using optimal USusing op
US processing
processing time,
time, with with model.
Weibull Weibull model.
3.2. Optimal Pre-Treatment Parameters
3.2. Optimal Pre-Treatment Parameters
The final dried products are shown in Figure 3. The change in color of the samples
The finalsignificant
was statistically dried products(from ∆E are shown
= 3.95 in for
± 0.98 Figure
samples3. The change
treated at 30%infor
color of the sam
30 min
was
to statistically
lowest color change ∆E = 3.35
significant (from
± 0.52ΔE for= samples
3.95 ± 0.98 for samples
treated at 90% fortreated at 30%5).for 30 m
60 min (Table
As the difference
lowest in the ΔE
color change color of the± samples
= 3.35 0.52 fortreated
samples during 30 and
treated 60 min
at 90% fortreatments
60 min (Table 5
at 90% amplitude was not statistically significant, a shorter processing
the difference in the color of the samples treated during 30 and 60 min treatments time seems to be at
more suitable. However, compared to the duration of ultrasound pre-treatment, it can be
amplitude was not statistically significant, a shorter processing time seems to be m
observed that the dried pumpkin was lighter (L*) after 45 and 60 min than after 30 min
suitable.
of sonication.However, compared
These results could betoexplained
the duration
by the offactultrasound pre-treatment,
that the ultrasound treatmentit can b
served
leads that the dried
to cavitation, whichpumpkin was lighter
causes a structural change(L*)in after 45 andresponsible
the enzymes 60 min than after 30 m
for the
sonication.brown
undesirable These results
color couldoxidases),
(polyphenol be explained by the fact
and consequently that the
inhibits thebrowning
ultrasoundof treatm
the pumpkin. The relation of ultrasonic parameters to the drying time
leads to cavitation, which causes a structural change in the enzymes responsible is presented in Table 6. fo
As expected, the drying time without ultrasound treatment was the longest (452 min), and
undesirable brown color (polyphenol oxidases), and consequently inhibits the brow
it can be observed that each ultrasound parameter tested significantly reduced the drying
of the pumpkin. The relation of ultrasonic parameters to the drying time is presente
time. A possible consequence of the mechanical and thermal effects of cavitation on all
Table 6.
treated As expected,
samples the drying
is the change time without
of the pumpkin matrix andultrasound treatment
consequently was the longest
the enlargement
min),
of and itItcan
the pores. alsobe observed
leads that each
to a decrease in theultrasound
adhesion of parameter
water molecules tested significantly
bound to the red
thewalls
cell drying[38].time. A possible
Numerous studies consequence
have reported that of the mechanical
cavitation phenomenaand cause
thermal effects of ca
a change
in the on
tion structure of the samples
all treated product and in this
is the way facilitate
change the faster removal
of the pumpkin matrix of moisture
and consequently
from the product. Liu et al. reported how the microstructure of purple-fleshed sweet
enlargement of the pores. It also leads to a decrease in the adhesion of water mole
potatoes changed after ultrasonic treatment, showing more microchannels and expanded
bound to the
intercellular cell Chao
spaces. wallset[38]. Numerous
al. also confirmed studies have reported
that ultrasound that significantly
pretreatments cavitation phenom
cause a change
accelerated in the
the drying ratestructure
of seed-usedof the product
pumpkin dueand in this waydestruction
to cell-structure facilitate [46–49].
the faster rem
A larger number of larger pores also leads to an increased mass transfer of water during
drying and shortens the drying time.
 of moisture from the product. Liu et al. reported how the microstructure of purple
sweet potatoes changed after ultrasonic treatment, showing more microchannels
panded intercellular spaces. Chao et al. also confirmed that ultrasound pretreatm
nificantly accelerated the drying rate of seed-used pumpkin due to cell-structure
Processes 2023, 11, 469 tion [46–49]. A larger number of larger pores also leads to an increased mass tra
8 of 13

water during drying and shortens the drying time.

Figure3.3.Dried
Figure Driedpumpkin
pumpkin slices.
slices. (A–C)—30%
(A–C)—30% amplitude,
amplitude, 30, 45 30,
and4560and
min60 min processing
processing time; time
90% amplitude, 30, 45 and 60 min, respectively.
(D–F)—90% amplitude, 30, 45 and 60 min, respectively.

Table
Table Relationship
5. 5. between
Relationship ultrasonic
between parameters
ultrasonic and color change
parameters in samples.
and color change in samples.
US Power/% Sonication Time/min Total Color Change/∆E
US Power/% Sonication Time/min Total Color Change/ΔE
30 30 3.95 ± 0.98a
3030 45 30 3.95 ± 0.98a
4.11 ± 1.19b
3030 60 45 3.87 ± 0.55a
4.11 ± 1.19b
6030 30 60 4.26 ± 0.12b
3.87 ± 0.55a
60 45 4.18 ± 1.07b
6060 60 30 4.26 ± 0.12b
4.17 ± 1.12b
9060 30 45 4.18 ± 1.07b
3.63 ± 0.58a
90 45 3.40 ± 0.57c
90
60 60
60 4.17 ± 1.12b
3.35 ± 0.52c
90
abc—different superscript letters within columns30
are significantly different (p < 0.05). 3.63 ± 0.58a
90 45 3.40 ± 0.57c
Table 6. Relationship between the ultrasonic parameters and drying time.
90 60 3.35 ± 0.52c
US Power/%
abc—different Sonication
superscript Time/min
letters within Drying Time/min
columns are significantly different (p < 0.05).
0 0 451.67 ± 7.64a
30 30 361.67 ± 2.89b
The 30
statistical analysis of45the studied ultrasound parameters, shown in Figu
356.66 ± 2.89c
vealed that
30 the shortest drying 60time was obtained at 351.67
a maximum
± 2.89c ultrasound amp
90% for 4560 min. With these parameters,
30 the water content
358.33 ±in the samples after dry
2.89b
8%, which 60 is within the expected
45 346.67 ± 2.89c
range. Further increasing the processing time
60 60 343.33 ± 2.89c
statistically significant effect on the drying time nor caused an additional redu
90 30 349.00 ± 5.00d
water content.
90 45 322.33 ± 2.89e
90 60 320.67 ± 2.89e
Table 6. Relationship
abc—different between
superscript letters the ultrasonic
within columns parameters
are significantly different (p <and
0.05).drying time.

USstatistical
The Power/% analysisSonication Time/min
of the studied DryinginTime/min
ultrasound parameters, shown Figure 2,
revealed that0the shortest drying time was0 obtained at a maximum ultrasound451,67amplitude
± 7,64a
of 90% for 45 min. With these parameters, the water content in the samples after drying
30 30 361.67 ± 2.89b
was 8%, which is within the expected range. Further increasing the processing time had
30significant effect on the drying
no statistically 45 356.66
time nor caused an additional ± 2.89c
reduction in
water content.30 60 351.67 ± 2.89c
One factor that had an impact on the longer drying times that correlated with the longer
60 30 358.33 ± 2.89b
processing times was the initial greater mass of water after processing, and consequently,
before drying.60This may be related to the45
phenomenon of water penetration346.67
into the±cellular
2.89c
60 60 343.33 ± 2.89c
90 30 349.00 ± 5.00d
 the cellular structure of the samples due to disequilibrium processing (as in the ex
process where ultrasound is widely used). A higher water content of the sample
60 min treatment compared to a 30 or 45 min treatment may significantly incr
Processes 2023, 11, 469 drying time, and there is no significant difference between samples 9treated of 13 for
and 60 min , regardless of amplitude. Figure 2 shows the comparison of drying
untreated samples and samples treated with the optimum processing paramet
structure
evidentofthat the both
samples due to disequilibrium
constant rate and falling processing (as in thewere
rate periods extraction process
affected by the u
where ultrasound is widely used). A higher water content of the samples
treatment, confirming previous claims about the effects of cavitation on the matrix after a 60 min
treatment compared to a 30 or 45 min treatment may significantly increase the drying
ing the microstructure, and increasing mass transfer rates. The optimal paramete
time, and there is no significant difference between samples treated for 45-min and 60 min,
mined for
regardless of ultrasonic treatment
amplitude. Figure arethe
2 shows consistent
comparison with the results
of drying time forofuntreated
other studies o
sonic drying.
samples and samplesSoquetta
treatedet with
al. show that ultrasonic
the optimum processingpretreatment
parameters. Itsignificantly
is evident cha
that both time
drying constantof rate and
beets duefalling rate influence
to the periods were ofaffected by the ultrasonic
the released mechanical treatment,
and therma
confirming previous claims about the effects of cavitation on the matrix, changing the
on the structure of the beets [46]. Jarahizadeh et al. showed that the application
microstructure, and increasing mass transfer rates. The optimal parameters determined for
sound has
ultrasonic a significant
treatment effectwith
are consistent onthetheresults
constant rate
of other period
studies during drying,
on ultrasonic drying. whic
related et
Soquetta toal.the increase
show in the mass
that ultrasonic diffusion
pretreatment rate duechanges
significantly to the the
enlarged pores
drying time of caused
beets due to the influence of the released mechanical and thermal
itation [49]. This phenomenon, caused by cavitation bubbles, results from energy on the structure of the fo
the beets [46]. Jarahizadeh et al. showed that the application of ultrasound
of microchannels and potential changes in the cell membrane and proves to be int has a significant
effect on the constant rate period during drying, which is also related to the increase in the
when
mass large amounts
diffusion rate due to of
thewater
enlarged need tocaused
pores be removed from[49].
by cavitation pumpkins or other fruits a
This phenomenon,
etables
caused by[50].
cavitation bubbles, results from the formation of microchannels and potential
changes in the cell membrane and proves to be interesting when large amounts of water
need
3.3. to be removed
Artificial fromNetworks
Neural pumpkins or other fruits and vegetables [50].

After Neural
3.3. Artificial testing different
Networks transfer functions, both neural networks were obtain
multilayer perceptron
After testing with the
different transfer BFGS training
functions, algorithm.
both neural networks wereThe ANN-1 network for
obtained using
multilayer
parameters perceptron
(90% forwith
45the BFGS
min) trainingof
consists algorithm.
10 hidden Theneurons,
ANN-1 network
with aforvalidation
optimal perfo
parameters (90% for 45 min) consists of 10 hidden neurons, with a validation
of 0.999991. The mean square error was 9.02 × 10 . It is evident that the MSE w
−6 performance
of 0.999991. The mean square error was 9.02 × 10−6 . It is evident that the MSE was much
lower compared to the Weibull model, as shown in Figure 4, indicating a better
lower compared to the Weibull model, as shown in Figure 4, indicating a better fit than any
any
of the of the analyzed
analyzed mathematical
mathematical models. Thismodels. Thiswith
is consistent is consistent with studies
studies by various authors by var
thors who have compared ANN with empirical models [51,52].
who have compared ANN with empirical models [51,52].

Figure
Figure 4. 4. Comparison
Comparison of fitting
of fitting of ANN-1
of ANN-1 andmodel
and Weibull Weibull modelvstopredicted
to observed observed vs predicted
values. va
The ANN-2 network, consisting of 15 neurons in hidden layers, had a performance
of 0.999987. The mean square error was 8.03 × 10−5 . It can be concluded that artificial
neural networks can be successfully used to model the drying process in combination with
ultrasound pretreatment. Moreover, both ANNs (Figures 4 and 5) were significantly more
accurate than the standard empirical models tested. It should be taken into consideration
 The ANN-2 network, consisting of 15 neurons in hidden layers, had a perfo
of 0.999987. The mean square error was 8.03 × 10−5. It can be concluded that artificia
networks can be successfully used to model the drying process in combination wi
Processes 2023, 11, 469
sound pretreatment. Moreover, both ANNs (Figures 4 and 5) were significantly 10 of 13
m
curate than the standard empirical models tested. It should be taken into consi
that empirical models such as Weibull were based on only one set of process par
while
that the significantly
empirical models such better ANN-2
as Weibull network
were based considered
on only one set of all process
process parameters a
parameters,
This the
while shows that ANN-2
significantly can successfully
better ANN-2 predict
network considered allthe effects
process of all tested
parameters process v
as inputs.
This shows that ANN-2 can successfully predict the effects of all tested
on the drying time/moisture ratio, thus eliminating the need for multiple mod process variables on
the drying time/moisture ratio, thus eliminating the need for multiple models that could
could become useless even with minor changes in the drying process. Due to the
become useless even with minor changes in the drying process. Due to the minimal errors
errors
and R2 >and
0.999,Rboth
2 > 0.999, both ANN models can replace mathematical models for ul
ANN models can replace mathematical models for ultrasonic drying
drying
of pumpkinof slices,
pumpkin slices,
regardless regardless
of the of the process
process parameters used. parameters used.

Figure
Figure 5. 5. Fitting
Fitting of ANN-2
of ANN-2 to experimental
to experimental data. data.
4. Conclusions
4. Conclusions
The drying of pumpkin pulp using ultrasonic pretreatment shows that increasing
The power
processing dryingbyofuppumpkin pulp using
to 90% significantly ultrasonic
reduces pretreatment
drying time. An increaseshows
in the that in
ultrasonic processing time negatively influences the drying process,
processing power by up to 90% significantly reduces drying time. An increase iso that prolonging
drying time beyond 45 min only leads to increasing energy costs. The performed analysis
trasonic processing time negatively influences the drying process, so that prolong
of the mathematical models shows that the Page model has the best fit for drying the
ing timesamples,
untreated beyond 45 min
while only leads
the Weibull model to
hasincreasing energy
the best fit for costs. The
the ultrasonically performed an
pretreated
the mathematical models shows that the Page model has the best
dried samples. This model can further be used as a basis for estimating drying parameters fit for drying
and potentially
treated for the
samples, design
while of Weibull
the ultrasonic model
drying processes or equipment.
has the best Color
fit for the change
ultrasonically pr
of samples was evident, but minimal. The lowest color change was obtained using optimal
dried samples. This model can further be used as a basis for estimating drying par
processing parameters. However, the best fit to the process parameters was obtained using
and
the potentially
artificial for the design
neural network, which wasof found
ultrasonic drying
to be more processes
accurate or equipment.
in predicting the effects Color
ofprocess
of samples was evident,
parameters but minimal.
on the drying process. The lowest color change was obtained using
processing parameters. However, the best fit to the process parameters was obta
Author Contributions: Conceptualization, S.K. and F.D.; methodology, A.N.G.; software, S.K. and
ing the artificial neural network, which was found to be more accurate in predic
F.D.; formal analysis, M.B.S. and A.N.G.; investigation, M.Š. and M.A.Š.; writing—original draft
effects ofS.K.
preparation, process parameters
and F.D.; onand
writing—review theediting,
drying process.
S.R.B. and M.B.S.; supervision, M.B.; project
administration, M.B.; funding acquisition, M.B. All authors have read and agreed to the published
version
Author of Contributions:
the manuscript. Conceptualization, S.K. and F.D.; methodology, A.N.G.; softw

and F.D.;
Funding: Theformal
work wasanalysis,
supported M.B.S. and A.N.G.
by the Croatian ; investigation,
Science M.Š.project
Foundation (Research and M.A.Š. ; writing
“Hybrid
drying and valorization of plant food waste and by-products”) IP-2019-04-9750-HYDRYBY.
nal draft preparation, S.K. and F.D.; writing—review and editing, S.R.B. and M.B.S
Institutional
vision, M.B. Review
; project Statement: Not applicable.
Boardadministration, M.B.; funding
acquisition, M.B. All authors ha
and agreed
Informed to Statement:
Consent the published version of the manuscript.
Not applicable.

Funding: The work was supported by the Croatian Science Foundation (Research project
drying and valorization of plant food waste and by-products”) IP-2019-04-9750-HYDRYB
Processes 2023, 11, 469 11 of 13

Data Availability Statement: The data that support the findings of this study are available from the
corresponding author, M.B., upon reasonable request.
Conflicts of Interest: The authors declare no conflict of interest.

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