Biomass Conversion and Biorefinery

https://doi.org/10.1007/s13399-023-04269-8

ORIGINAL ARTICLE

Effect of ultrasound pretreatment and drying air temperature

on the drying characteristics, physicochemical properties,
and rehydration capacity of raisins
Ahmet Candemir1 · Gülşah Çalışkan Koç2 · Safiye Nur Dirim3 · Ravi Pandiselvam4

Received: 4 January 2023 / Revised: 22 April 2023 / Accepted: 24 April 2023

© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2023

Abstract
One of the most significant dried foods is raisin, used directly as ingredients in confectionary and in the form of raisin paste
used in sauces, fillings, baked goods, microwaveable coatings, and other culinary products to color them naturally. The
purpose of this study is to investigate the effects of ultrasound pretreatment (53 kHz, 300 W, 30 °C, 300 s, in a mixture of
5% ­K2CO3+ 1% OO solution) and drying air temperatures (40–60 °C) on the drying behavior, color values, physicochemi‑
cal properties (moisture content, VCC, TPC, RSC, and antioxidant capacity (DDPH)) and rehydration capacity of Sultani
Çekirdeksiz grapes. Both the drying kinetic (drying time, drying rate, and effective moisture diffusivity) and the quality
characteristics of grapes were significantly improved by ultrasound pretreatment (p < 0.05). In addition, the vitamin C
(0.75–3.86 mg/g) and total phenolic content (1.31–1.80 mg GA/kg) of raisins were highly protected with the high drying
temperature and ultrasound pretreatment. The antioxidant capacity (1.15–5.50 mM Trolox) of samples increased with drying
temperature whereas the antioxidant capacity decreased with ultrasound application. The rehydration time of all samples
was found around 800 min. As a result of this study, it can be said that the ultrasound application may be used successfully
for drying grapes and that a greater degree of the nutritional value of the grapes can be maintained.

Keywords Grape · Ultrasound pretreatment · Hot air drying · Total phenolic content · Antioxidant capacity

Nomenclature
AC Antioxidant capacity
* Ravi Pandiselvam
anbupandi006@gmail.com; r.pandiselvam@icar.gov.in a* Redness/ Greenness
ANOVA Analysis of variance
Ahmet Candemir
ahmetcandemir.dem@gmail.com b* Blueness/ Yellowness
DDPH 1,1-diphenyl-2-picrylhydrazyl
Gülşah Çalışkan Koç
gulsahcaliskan86@gmail.com; gulsah.koc@usak.edu.tr Deff Effective Moisture Diffusivity
­(m2/s)
Safiye Nur Dirim
nur.dirim@ege.edu.tr DM Dry matter
D0 Pre-exponential factor ­(m2/s)
1
Viticulture Research Institute, Manisa, Turkey DR Drying rate
2
Food Technology Program, Food Processing Department, dt Drying time (min)
Eşme Vocational School, Uşak University, Eşme, Ea Activation energy (kJ/mol)
Uşak 64600, Turkey
FRAP Ferric reducing antioxidant power
3
Engineering Faculty, Department of Food Engineering, Ege assay
University, Bornova, Izmir, Turkey
g Gram
4
Physiology, Biochemistry, and Post‑Harvest Technology GA Gallic acid
Division, ICAR-Central Plantation Crops Research Institute h Hours
(CPCRI), Kasaragod, Kerala 671124, India
HA (°) Hue angle

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 Biomass Conversion and Biorefinery

HAD-40°C-US-P Hot air dried at 40 °C, ultrasound 1 Introduction

pretreated sample
HAD-40°C-NON-P Hot air dried at 40 °C, untreated The short harvest period of several fruits and vegetables
sample brings about the necessity of drying to have longer shelf
HAD-50°C-US-P Hot air dried at 50 °C, ultrasound lives. In the case of grapes, this fact is also valid. In addition,
pretreated sample the most common usage of grape is in raisin form. The
HAD-50°C-NON-P Hot air dried at 50 °C,untreated primary goal of drying is to lower the moisture content to
sample act against microbiological contamination and enzymatic
HAD-60°C-US-P Hot air dried at 60 °C, ultrasound response. In the food processing industry, additional
pretreated sample advantages can be listed as long shelf lives, reduced
HAD-60°C-NON-P Hot air dried at 60 °C, untreated transportation costs, reduced need for the storage area,
sample ready to eat high nutrition snacks, and ready additives for
K2CO3 Potassium carbonate food processing. On the other hand, drying requires a lot of
kHz Kilohertz time and energy and typically has a negative effect on the
L Liter quality of the product. Because of this reason, the effect of
L* Lightness drying circumstances impacts on color, texture, rehydration
L/s Liter/second potential, nutritional value, and sensory quality must be
ln Natural logarithm assessed before choosing the drying technique [1].
m/s Meter/second There are three primary techniques for drying grapes:
mg Milligram sun drying, drying in the shade, and drying with various
ml Milliliter industrial dryers. Most cultivated grapes are typically dried
MR Moisture ratio by sun exposure. However, this practice has drawbacks,
Mee Equilibrium moisture content including lengthy drying durations, environmental pollution
Mt Moisture content at any time from dust and insect infestations, microbial contamination
M0 Moisture content at the beginning from rain, and color deterioration from solar radiation.
NaOH Sodium hydroxide Additionally, after gathering dried raisins, a cleaning
m Weight of the sample (g) procedure is required to remove impurities [2]. The drying
min Minute of grapes is mainly composed of pretreatment, drying, and
Mt Moisture content at any time t (kg post treatments. The primary pretreatment commonly used
water/kg DM) in Turkey is dipping into an olive oil solution containing
Mt+dt Moisture content at time t + dt ( kg potassium carbonate. Other remedies include soaking in
water/kg DM) hot water or applying chemicals like caustic, sulfur, ethyl,
nm Nanometer or methyl oleate emulsions [3]. Using potassium carbonate
NON-P Untreated samples solution creates micro fissures that cause waxes and lipids to
OO Olive oil be eliminated, grape skin cells to collapse, and a partial loss
PCA Principal component analysis of intracellular connections [4]. Additionally, the potassium
R Gas constant (8.31451 J/mol K) carbonate can increase water loss by neutralizing free fatty
R2 Correlation coefficient acids and fixed charges on the surface of the fruit [5]. The
RSC Reducing sugar content treated grapes are mostly sun-dried on concrete surfaces and
s Second sometimes on a canvas sheet. The reason for the need for
t Time (s) pretreatment for the grapes is due to the waxy and layered
T Absolute temperature (K) skin of the berries, which controls the rate of moisture
TPC Total phenolic content diffusion and prolongs the drying time. There might be
TS Turkish standart some losses in the quality attributes due to long drying times
US-P Ultrasound pretreated with low-moisture diffusivity or the need for high drying
UV Ultraviolet temperatures. The waxy nature is advantageous because it
VCC Vitamin C content shields the fruit from fungi, UV rays, and physical harm. In
v:v Volume: volume addition, as the waxy layer significantly influences the safety
W Watt of the dried product and shelf life in the skin, its removal
wb Wet basis calls for extra care. The dried grapes are usually stored in
w:v Weight: volume uncontrolled conditions for long times and require another
w:w Weight: weight cleaning or sorting process [6]. Additional pretreatments
ΔE Total color change

13
Biomass Conversion and Biorefinery
can be a proper solution to increase the shelf-life quality of
the dried grapes. In the literature, in addition to chemical
methods, some other treatment methods like microwave
heating, ohmic heating, or superficial abrasion of berries
have been mentioned. The ultrasound treatment, which has
been used in the drying of many fruits and vegetables, is
another possible method that may suit for processing of
grapes [7].
The ultrasound application may overcome some
disadvantages of convective drying by boosting the drying
rate at lower temperatures and, thereby, the mass transfer
phenomenon. By alternating between expansion and
compression cycles, the mechanical energy generated by
the use of power ultrasound helps to lower both internal and
external barriers (sponge effect) to mass transfer, with water
transfer being significantly improved. The use of ultrasound
in osmotic dehydration suggests that grapes may be dipped
using ultrasound [8]. For this reason, applying ultrasound in
olive oil solution containing potassium carbonate as a dipping
pretreatment becomes a feasible alternative. The practical
advantages of ultrasound can be defined as being applicable
continuously or intermittently, and temperature control can
be applied during the process [9]. It has been reported in all
the studies where ultrasound is applied that the ultrasound
application decreases the drying time, increases the effective
moisture diffusivity values, and decreases the energy
utilization for the overall drying process, but it also may have
a negative effect as the mass exchange in the fluid where the
application is performed [10]. However, this disadvantage
might be eliminated since grapes have waxy and layered skins.
Studies on the impact of ultrasonic pretreatment in the
drying of numerous fruits are found when the studies in the
literature are studied. The studies have examined how ultra‑
sound affects the drying kinetics of grape stalks [11] and
grape seeds [12]. However, no study covers the pre-applica‑
tion of ultrasound in grape drying. Studies generally focus
on how ultrasonic treatment affects the extraction of valuable
components from grapes. The objective of this study is to
determine the drying behavior of grapes and some specific
biochemical characteristics that are affected by ultrasonic
pretreatment. As far as we know, this is the first study in
which grapes were dipped into an olive oil solution contain‑
ing potassium carbonate while an ultrasound application was
used.
2 Material and methods
2.1 Materials
The Sultani Çekirdeksiz grape variety, harvested by
Manisa Viticulture Research Institute Directorate (Manisa,
TURKEY) in August 2016, was used. Manisa Province is
located between 27°6′58″ and 27°39′41″ east longitudes,
38°27′17″ and 38°55′55″ north latitudes. Sultani Çekirdeksiz
grapes were harvested when they reached 22–23% water-
soluble dry matter value by following their maturity.
Grapes were kept at refrigeration conditions (4 °C) until
drying studies at the Ege University, Department of Food
Engineering, Turkey. Gallic acid, (±)-6-hydroxy-2,5,7,8-
tetramethychromane-2-carboxylic acid (Trolox), and Folin-
Ciocalteu reagent, 1,2-diphenylpicrylhydrazyl (DPPH) were
purchased from Sigma Aldrich (St Louis, USA). Other
solvents and reagents were analytical grades.
2.2 Method
2.2.1 Ultrasound pretreatment
Grape samples were separated as 5 kg lots and subjected
to ultrasound pretreatment in the specified dipping solution
(5% ­K2CO3 + 1% OO solution, 5.1±0.1°Bx measured by
HANNA HI 96,801, USA), which is applied to remove
the outer waxy layer from the grapes before drying. The
ultrasound pretreatment was performed at 53 kHz frequency,
300 W ultrasound power, 30 °C temperature, and 300 s of
application time. Ultrasound applications were carried out
in an ultrasonic water bath (Kudos, SK7210HP, Turkey),
and the grape to solution ratio was kept constant at 1:4
(w:w). Control samples were also immersed in the solution
(a mixture of 5% ­K2CO3+ 1% OO) for 5 s, but ultrasound
pretreatment was not applied.
2.2.2 Hot air drying
An airflow tray dryer (Uop8-A, Armfield Ltd., UK, 1 m/s air
flow rate, 40, 50, and 60 °C temperatures) was used to dry
grapes (5 kg) with and without ultrasound pretreatment [3].
The weight of samples was measured every 10 min during
drying. All weight measurement processes were completed
in the possible shortest time (max. 5 s) to maintain the
drying regime. The drying process was continued until a
constant weight was achieved. Dimensionless moisture
(contents content
) values in terms of moisture ratio
Mt−Me
MR = M0−Me were computed from the weight changes.
The final moisture content was accepted as equilibrium
moisture content. Before and following the drying procedure,
the weight of the grape sample was measured, and the drying
efficiency was computed by using the ratio of the final
weight of the dried sample to the initial weight of the fresh
sample (%). Drying rate, effective moisture diffusivity
(simplified Fick’s second law), and activation energy was
calculated according to Eqs. 1–5, respectively [13]. The
samples dried under different conditions are depicted in
Fig. 1
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 Biomass Conversion and Biorefinery

Fig. 1  Raisins dried under

under different drying system
and temperature

Mt+dt − Mt moisture content in an oven (FN-500 Nüve, Turkey) set at 70

DR = (1) °C. Using a water activity measurement tool (Testo AG 400,
dt
Germany) and a colorimeter (Konica Minolta Chroma Meter
M − Me
[ 2 Deff t
] CR-400, Japan), the water activity and color values (L*, a*,
8 ∑∞ 1 2𝜋
MR = = 2 exp −(2n + 1) and b*) of the grapes and raisins were measured. The Chroma,
M 0 − Me 𝜋 n=0
(2n + 1)2 4 L2
Hue Angle (°), and total color changes values were calculated
(2)
according to given Eqs. 6–8 [15].

For long drying times (MR < 0.6), a limiting case of Eq. (6)
√
Chroma = a∗2 + b∗2
(2) was assumed and expressed in the logarithmic form as
in Eq. 3 (
b∗
)
H(◦ ) = tan−1 (7)
( ) ( π2 D )
8 a∗
eff
lnMR = ln 2 − 2
t (3)
π 4L
(8)
√
ΔE = Δa∗2 + Δb∗2 + ΔL∗2
From Eq. 3, a plot of lnMR versus drying time gives a
straight line with a slope of Eq. 4 The sample preparation method developed by Baloch
et al. [16] and updated by Özkan [17], as well as the sample
π2 Deff preparation stages, was used to ascertain the degree of
Slope = (4)
4L2 browning. In addition, it has been reported that there is a
correlation between non-enzymatic browning and alcohol-
The relationship between the ­Deff and the air temperature
soluble color pigments. Therefore, alcohol-soluble color
was assumed to be the Arrhenius function and ­Ea was cal‑
index values were also determined to monitor the amount
culated using Eq. 5.
of non-enzymatic browning in raisins [18].
(
Ea
) The pH values were measured at room temperature using a
Deff = D0 exp − (5) pH meter (WTW InfoLab pH720, Germany). For the titrable
RT
acidity analysis, 10 ml of grape juice or the reconstituted
raisins to initial moisture content passed through a Whatman
2.2.3 Analysis No:1 filter paper and 10 ml of distilled water was placed on
the obtained aqueous sample and titrated with 0.1 N NaOH
The number of grains in 100 grams of sample and, until the pH was 8.1. The conversion factor is 0.075 for
accordingly, the size classification were determined according tartaric acid and the results were determined as grams of
to TS 3411 [14]. Fresh grapes and raisins were analyzed for tartaricacid per kg of raisins [19, 20].

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Biomass Conversion and Biorefinery

Vitamin C, reducing sugar, and total phenolic contents The at 10-min intervals. After removing excess water from the
method expressed by Cemeroğlu [18] was followed to deter‑ raisin, the raisin was weighed and immersed in the water
mine the VCC of raisins. First, the raisins were diluted to again, and the rehydration process continued until the mass
the initial moisture content and filtered (Whatman No:1 fil‑ of the samples reached the balanced (constant) weight.
ter paper) to take 10 ml. Then, the oxalic acid solution (90
ml of 0.04% oxalic acid/distilled water (w:v)) was added. Statistical analysis Two parallel runs of drying experiments
The sample solution (1 ml) was taken in one tube, 9 ml of and analyses were carried out. Six further color measure‑
distilled water (replicate solution) was placed on it, and 9 ments were taken. The SPSS 16.0 package program (SPSS
ml of dye solution (12 mg 2, 6dichloroindophenol/1 liter of Inc., USA) (ANOVA for temperature and independent
distilled water, sample solution) was placed in the other tube. sample t-test for ultrasound pretreatment) was used to test
The sample solution absorbance was determined at 518 nm the experimental results, which was presented as mean ±
absorbance as opposed to the replicate solution (Varian Cary standard deviation with a 95% confidence interval. Using
50 UV/Vis, Australia). The results were given as mg vitamin XLSTAT version 2010, Principal Component Analysis
C/g in raisins [y = 0.0217 × +0.0177 (R2 = 0.9944)] using (PCA) was carried out (Addinsoft, New York, NY).
the calibration curve. L-ascorbic acid (Carlo Erba Reagents)
was used to plot the standard curve.
The Lane-Eynon method was applied to determine the 3 Results and discussion
RSC of samples [20]. The TPC analysis was performed in
the first extraction and the second analysis. For the extrac‑ 3.1 Drying kinetics of the grapes
tion purpose, 100 g of raisins were mashed, and 5 g of sam‑
ple were taken. Then 20 ml of extraction solution, includ‑ The rate of change in MR of grapes with respect to drying
ing ethanol:water 80:20 (v:v), was added to the sample and time is given in Fig. 2a. Figure 2a shows that the samples
homogenized (IKA, Ultraturrax, T25, Germany). In the next with and without ultrasound pretreatment showed similar
step, samples were centrifuged (Nüve, NF400, Turkey) at
4100 rpm for 5 min. Then the aqueous solution was poured.
This cycle was executed two times. Then the test tube was
completed to 50 ml with extraction solution. Next, the analy‑
sis was modified, and 8 ml of extracted samples are com‑
bined into a test tube with 2 ml ­Na2CO2 solution (20%, w:v)
in water and 0.2 ml Folin-Ciocaltaeu reagent (10%, v:v, in
water) from the Sigma-Aldrich Corp. The test tube was then
left at room temperature for 2 h and the absorbance of the
solutions was measured at 760 nm using aspectrophotometer
(VarianCary 50 UV/Vis, Australia). From the standard graph
created using gallic acid, the TPC was reported as mg GA/
kg [y = 0.1507 ×  + 0.5494, (R2 = 0.9977)] [21].

Antioxidant capacity Antioxidant capacity analysis was per‑

formed using the modified Sanchez-Moreno method. First, the
samples were diluted to different concentrations. Then,a 0.1
ml sample of these solutions was placed in amber bottles, and
DPPH (1,1-diphenyl-2-picrylhydrazyl) solution prepared in
3.9 ml methanol with a concentration of 0.02 g/L was added.
After 40 min waiting period at room temperature, the absorb‑
ance values of the samples were measured using a spectropho‑
tometer (Carry 50 Scan, Varian) at 517 nm [22, 23]. For sam‑
ple solutions, the decrease in absorbance value (expressed as
a percent of initial absorbance value) gives percent inhibition
rates. Radical scavenging capacity was given as mM Trolox.

Rehydration capacity Raisins were placed in water at room

temperature at a ratio of 1:5 (w:w) raisins to water. The rai‑ Fig. 2  Moisture ratio versus drying time (a) and drying rate versus
sins were removed from the water with the help of a strainer moisture content (b)

13

drying behavior at the same drying temperature, except the
samples dried at 60 °C. Clemente et al. [9] also reported
that due to the structure of grape seeds (very hard and less
porous), applying ultrasound did not significantly alter the
drying kinetics of grape seeds. HAD-50 °C-NON-P, HAD-
60 °C-US-P, and HAD-60 °C-NON-P samples exhibited
convex decreasing curves. Convex decreasing curves are
very commonly observed curves in food drying. However,
the HAD-40 °C-US-P and HAD-40 °C-NON-P samples
exhibited concave decreasing curves. The tail was visible
in samples below the MR value of 0.4. In the case of HAD-
50 °C-US-P sample, a convex decreasing and concave tail‑
ing curve was observed [24].
The samples dried faster by raising the drying tempera‑
ture and using ultrasonic treatment (p < 0.05). When the
drying times of the samples are examined, it is seen that an
increase in temperature of 10 °C reduced the drying time
between 4.9 and 21.8 h. Due to the increased heat and mass
transfer rates at high temperatures, it is estimated that the
drying rate will increase and the drying time will decrease.
The drying times of the samples decreased by around 2.5
and 9.7 h as a result of ultrasound pretreatment. Microscopic
channels can express it in the material created by ultrasound
applications. These channels improve the water removal
from the material [25]. This is important in terms of both
the product being exposed to heat for a long time and the
termination of chemical reactions, as well as energy saving.
In another study, the drying times of seedless grapes were
reported as 2880 and 1080 min, respectively, for drying air
temperatures of 60 °C and 70 °C in a cabinet dryer. When
the samples were dipped into a solution of traditional potas‑
sium carbonate, prepared by dissolving 0.5 kg ­K2CO3 in 10
L of water and adding 0.05 kg OO, the drying times were
measured as 1320 and 870 min for the same conditions [3].
The ultrasound treatment (21.7 kHz, 45 W) decreased the
drying time of the convectively dried grape skin (70 °C, 1
m/s.) by about 6.6% [26]. Cruz et al. [26] stated that the
unique structure of the grape skin is responsible for the low
effect of ultrasound; however, in this study, ultrasound was
applied in the mixture of 5% K ­ 2CO3+ 1% OO solution as
pretreatment, and it is known that the use of this solution
accelerates the drying process by reducing the waxy feature
of the grape skin. Drying time decreased by around 9.2% in
samples dried at 40 °C, 4.8% in samples dried at 50 °C, and
21.3% in samples dried at 60 °C. Similarly, García-Pérez
et al. [11] reported that the ultrasound pretreatment (21.8
kHz, 45 and 90 W) decreased the drying time of convec‑
tively (40 °C) dried grape stalk by around 22% (45 W) and
28% (90 W). This decrease was lower at 60 °C: around 17%
and 22% at 45 W and 90 W. The drying efficiency values
of the samples ranged between 58.49 and 76.72%. Higher
drying efficiency values were obtained with lower drying air
temperatures and ultrasound application.
13
Biomass Conversion and Biorefinery
The drying rate values of the grapes were calculated and
plotted against the moisture content, as illustrated in Fig. 2b.
Drying generally took place in the falling rate period. Higher
drying rate values were seen at the beginning of the drying
process as expected, and these values decreased as the dry‑
ing time increased. It is important to note that even while
the high temperatures speed up the diffusion of water vapor,
the high driving force of mass transfer led to greater drying
rate values. In addition, high drying air temperatures can
decrease the relative humidity of the air, increase the mois‑
ture gradient between samples and air, and promote water
mobility within samples, thus resulting in higher drying
rates [27]. Similar findings, as the drying rate is increased
with an increase in temperature for seedless grapes were
also obtained by Çağlar et al. [28]. Higher drying rate val‑
ues were obtained for the ultrasound-pretreated samples.
This may be because the waxy layer on the surface of the
grape, which causes greater resistance to water vapor per‑
meability was damaged. Also, it is possible that ultrasound-
induced cell lysis promoted water outflow from the cell [10,
28, 29]. This situation can also be associated with shorter
drying time and effective diffusion coefficient compared to
untreated samples.
The ­Deff values were calculated from the slope obtained
by plotting the graph of ln MR versus ln time. Effective
moisture diffusivity values of ultrasound-pretreated hot air-
dried samples are 1.69*10−7 m/s2 (40 °C), 2.28*10−7 m/
s2 (50 °C), and 4.68*10−7 m/s2 (60 °C) and unpretreated
hot air-dried samples 1.66*10−7 m/s2 (40 °C), 2.16*10−7
m/s2 (50 °C), and 2.34*10−7 m/s2 (60 °C), respectively.
The effective moisture diffusivity values of infrared dried
(50–80 °C) with and without pretreatment (5% ­K2CO3 and
0.5% OO /1L water for 5 min) seedless grape was found as
5.39*10−10−2.09*10−11m/s2 [28]. Higher D ­ eff values were
obtained in this study. It may be due to different drying
techniques and conditions, grape variety, ultrasound appli‑
cation, etc. As expected, the effective moisture diffusivity
coefficient of the ultrasound-pretreated samples was higher
than the untreated samples. In addition, higher moisture dif‑
fusivity coefficient values were obtained at higher drying
temperatures since high air temperatures promote moisture
diffusion. Heating energy increases with temperature, and
this increases the activity of the water molecules leading to
higher moisture diffusivity [30]. The activation energy was
computed as 43.11 kJ/mol (R2 = 0.9381) and 14.67 kJ/mol
(R2 = 0.9231) for ultrasound pretreated and unpretreated
raisins, respectively. The results indicate that pretreated
raisins are more sensitive to temperature fluctuation than
unpretreated raisins. It is also reported that foods with high
sugar or pectin content, compact tissue structures, and small
specific surface area such as grapes may have higher activa‑
tion energy. In addition, pretreatments are effective on the
activation energy of grapes by changing the cell structure or
Biomass Conversion and Biorefinery

removing the waxy layer on the surface [30]. Similarly, in
this study, the ultrasound pretreatment was found effective
on the activation energy of grapes.
When the number of grains in 100 g of the samples is
examined (full data is not given), it is seen that the samples
dried at 40 °C are standard (US-P: 323, NON-P:347), and
the samples dried at 50 °C (US-P: 241, NON-P:236) and 60
°C (US-P: 175, NON-P:140) are jumbo. In addition, it can
be said that there are more grains in 100 g of ultrasound-
pretreated and low-temperature dried samples.
3.2 Physicochemical composition of the raisins
The pictures of raisins and the physicochemical composition
of the raisins are given in Fig. 1 and Table 1, respectively.
The moisture contents of raisins varied between 18.96 and
26.32%. Compared to samples subjected to ultrasound
pretreatment, it was discovered that the moisture content
of the untreated samples was relatively high (p < 0.05). The
moisture content of the samples reduced as the temperature
increased. The drying temperature and ultrasound
application generally affected the moisture value of the
samples (p < 0.05). However, the application of ultrasound
did not make a statistically significant difference in the
moisture content of the samples dried at 40 °C (p > 0.05).
The moisture content values of hot air (60 °C, 2 m/s, 19
h), vacuum (60 mbar, 2 L/s, 17.5 h), ultrasound-assisted
vacuum (60 mbar, 2 L/s, 20 kHz, 36 h), and freeze-dried
(−80 °C, 72 h) black “Isabel” grapes were found as 20.05 ±
0.70%, 20.00 ± 0.50%, 19.15 ± 0.49%, and 25.16 ± 0.76%,
respectively [25]. The moisture content values obtained
from this study showed similarity with the results obtained
by Ozkan et al. [25].
The water activity of the grape was 0.998. The drying
temperature and the ultrasound pretreatment were found
to have a significant impact on the water activity values (p
< 0.05). The water activity value of the samples dropped
with the application of ultrasound, reflecting the results for
moisture content (p < 0.05). Additionally, it was found that
grapes dried at 50 °C had the lowest water activity value,
while those dried at 40 °C had the highest water activity
value. It is possible that the crust that formed in the samples
as they dried at 60 °C stopped the water from leaving the
samples, increasing the water activity value.
Color is a critical factor for the acceptability of foods.
Visual appearance and color intensity of the food increased
by ultrasound application. All of the samples were light-
red in color, making it difficult to distinguish between them
(Fig. 1). As a result, color values (L*, a*, and b*) were
measured using a colorimeter (Table 1), and the chroma,
HA (°), and total color change values were calculated using
Eqs. 6–8. The color values of fresh grapes were measured
as L* = 45.56, a* = −1.90, and b* = 9.68. With the hot air
drying process, L* and b* values decreased while a* value

Table 1  Physicochemical composition of raisins

Analysis Convective hot air drying
40 °C 50 °C 60 °C
US-P NON-P US-P NON-P US-P NON-P

Moisture content (%, wb) 23.68±1.26ay 26.32±2.41az 19.02±0.98ax 22.32±2.41bx 18.96±1.26ax 21.52±2.19by
Water activity 0.734±0.060az 0.744±0.004bz 0.607±0.009axz 0.616±0.007ax 0.624±0.070 ay
0.658±0.009 by
Color
L* 33.57±1.27ax 33.41±0.89ax 30.72±2.23ax 32.36±1.87ax 30.42±2.74ax 31.86±1.98ax
a* 3.70±0.11bz 3.31±0.07az 2.49±0.19ay 3.48±0.02by 2.17±0.07ax 2.48±0.04bx
b* 4.59±0.09bz 3.85±0.14ay 2.36±0.08ay 3.76±0.07by 2.01±0.01ax 2.34±0.09 bx
Chroma 5.89±0.07az 5.08±0.02ay 3.43±0.17ay 5.12±0.19by 2.96±0.17ax 3.41±0.06 bx
HA (°) 51.13±1.05ay 49.31±2.27ay 43.46±1.04ax 47.21±0.98by 42.81±1.16ax 43.34±0.71ax
ΔE 14.18±0.12ax 14.45±0.04bx 17.12±1.01by 15.44±0.29ay 17.45±1.19ay 16.15±0.26az
pH 4.58±0.16ax 4.38±0.06ax 5.53±0.09 by 5.34±0.06 ay 5.53±0.04 ay 5.44±0.09 ay
Titratable acidity (tartaric acid g/kg, wb) 2.75±0.08bz 2.30±0.11az 1.05±0.02bx 1.00±0.01ax 1.25±0.03 by 1.10±0.04 ay
Vitamin C content (mg/100g, wb) 0.83±0.07ax 0.75±0.09ax 1.46±0.09by 0.88±0.12ax 3.86±0.19bz 3.02±0.26ay
Reducing sugar content (g/kg, wb) 411.42±33.93bx 371.23±7.97ax 536.41±87.23 ay 625.14±72.01 by 662.30±63.45az 689.69±20.60ay
Total phenolic content (g GA/kg, wb) 1.44±0.04bx 1.22±0.17ax 1.46±0.59ax 1.31±0.19ax 1.80±0.22 ay 1.77±0.49 ay
Radical scavenging activity 1.15±0.13ax 1.82±0.06bx 2.02±0.02 ay 3.40±0.21 by 5.23±0.47az 5.50±0.23az
(mM Trolox, wb)
a-b shows the statistical difference between the ultrasound pretreated and untreated samples (p < 0.05)
x-y shows the statistical difference between the different drying temperatures (p < 0.05)

13

increased both for the ultrasound treated anduntreated sam‑
ples. It can be claimed that the color values (L*, a*, and
b*), chroma, and HA (°) significantly decreased depending
on the drying temperature (p < 0.05). In addition, generally
higher total color change values were observed at higher
drying temperatures (p < 0.05). Non-enzymatic browning
reactions, the depigmenting effect of high temperature on
color pigments, etc., might cause this. Chroma, which is
thought of as the quantitative feature of colorfulness, and
humans increasingly perceive the color intensity of samples
with higher chroma values. HA (°), which is regarded as the
qualitative property of color, is the attribute that has gener‑
ally been used to identify colors as reddish, greenish, etc.
[15]. The chroma and HA (°) values changed between 2.96-
5.89 and 42.81-51.13, respectively. The lowest values were
obtained from HAD-60 °C-US-P sample, whereas, the high‑
est values were observed from HAD-40 °C-US-P sample.
It can also be stated that ultrasound application generally
caused a decrease in the color values and chroma and HA
(°) values except for 40 °C drying temperature (p < 0.05).
The total color change values were found to be higher than
14. It can be stated that the differences in perceivable color
can be analytically classified as very distinct (ΔE > 3 [31]).
The pH value of the fresh grape was 3.96. The pH values
of raisins were found to be higher than fresh grapes. Also, the
pH values of the ultrasound-pretreated samples were slightly
higher than thoseof no pretreatment applied. Generally, an
increase in pH was observed as the temperature increased
(p < 0.05). This may have resulted from the evaporation of
some organic acids during drying at high temperatures. Also,
according to the results, it can be said that the ultrasound
application has no significant effect on the pH value (p >
0.05), while the temperature is important (p < 0.05).
The grape had a titratable acidity of 6.23 g tartaric acid/kg.
The titratable acidity value of raisins significantly decreased
due to the drying procedure. Temperature and ultrasonic
pretreatment were statistically significant, according to the
analysis of the titratable acidity values (p < 0.05). The titrat‑
able acidity values decreased when the temperature was raised
from 40 to 50 °C, and they increased when the temperature
was raised from 50 to 60 °C (p < 0.05). It was shown that
samples subjected to ultrasound pretreatment had higher titrat‑
able acidity than untreated samples (p < 0.05). A graph of pH
versus titratable acidity was drawn to determine the relation‑
ship between the pH and titratable acidity of the samples.
As expected, the pH and titratable acidity content of ultra‑
sound pretreated (y = −1.6842 × +10.464, R2 = 0.9884) and
untreated (y = −1.2213 × +7.6383, R2 = 0.9763) samples
showed inverse relationship (Graph was not given).
The ultrasound application and drying temperature had
a significant (p < 0.05) impact on theVCC of raisins. Ultra‑
sound pretreatment and high-temperature drying resulted
in higher VCC (p < 0.05). The quick drying time at high
13
Biomass Conversion and Biorefinery
temperatures and the use of ultrasound may cause this situ‑
ation. Thus, the samples may have been exposed to heat
for a shorter time, and the loss of vitamin C may have been
less. According to Frias et al. [32], when compared to con‑
vective air drying (40–65 °C; 2–6 *10–1 m/s), ultrasound
drying (20 kHz; 100 W cm/s; 1.2 m/s; 120 mba; 1.6 kg/cm;
20–60 °C) led to greater vitamin C retention (55–92%) in
the carrots. In addition, Frias et al. [32] observed that the
vitamin C retention of ultrasound dried carrots is 55% at all
drying temperatures (20–60 °C). However, some researchers
reported that the higher drying temperatures caused higher
vitamin C loss due to oxidation and thermal degradation
[30, 32–34]. In addition, Gamboa-Santos et al. [34] reported
that the ultrasound application resulted in higher vitamin C
losses in the strawberries due to the air penetration in the
sample by ultrasound treatment.
An increase in the observable amount of RSC was
detected with the increase in the drying temperature (p
< 0.05). Except for those dried at 40 °C, the RSC of the
ultrasound-pretreated samples was lower than the sample
ultrasound not applied (p < 0.05). Jacob et al. [35] reported
that ultrasound application caused a slight decrease in the
sugar content of the mature coconut water due to the reduc‑
tion of browning in the ultrasound-treated samples. In addi‑
tion, it was reported that the RSC of mature coconut water
increased by ultrasound application (high shear force upon
cavitation) because of the release of entrapped sugar mol‑
ecules from the cell wall and membrane structure.
The phenolic content of fresh grapes was 524.01 mg GA/
kg. The phenolic content of raisins increased with increasing
drying temperature (p < 0.05). Cruz et al.[26] also revealed
that an increase in the drying temperature (40–70 °C) resulted
in higher phenolic content due to the less activity of the poly‑
phenol oxidase, which is responsible for polyphenol oxida‑
tion. Similarly, in this study, higher TPCs were observed at
higher temperatures. It was also determined that the TPC was
higher in the ultrasound-pretreated samples (p < 0.05). The
significantly lower drying time of ultrasound-pretreated sam‑
ples may be the reason for the higher TPC. Similarly, Ozkan
et al. [25] reported that higher phenolic losses were observed
at the ultrasound-assisted vacuum-dried raisins due to the
long drying time (almost twice longer as hot air and vacuum),
which causes the polyphenol oxidase release because of the
structural modifications and degraded cell wall. In addition,
Aydar et al. [36] reported that the highest TPC of Inula vis-
cosa (L.) was observed at maximum ultrasound pretreatment
(30 min,37 kHz, 150 W) and lowest microwave drying time
(1 min). The researchers claimed that applying ultrasound and
microwave might cause the higher extraction efficiency of the
phenolic compounds. However, longer microwave application
times may also destroy the phenolic compounds. Similarly,
Ren et al. [37] reported that ultrasound (20 kHz, 24.4–61 μm
amplitude levels for 1–5 min) pretreatment increased the total
Biomass Conversion and Biorefinery
phenolic, flavonoid, and quercetin contents, and antioxidant
activity (DPPH and FRAP) of hot air or freeze dried onion
slices. Researchers claimed that it may be due to the higher
extractability of these compounds induced by cavitation and
high shear forces resulting in increased mass transfer. How‑
ever, prolonged exposure time (> 3 min) reduced the TPC
and antioxidant activities due to the leaching of soluble bioac‑
tive compounds in the treatment solution through the micro‑
spores, oxidation, and thermal degradation in the presence of
an open atmosphere. Another reason may be due to the higher
impingement ability of ultrasound application to catabolize
cellular constituents that led to the acceleration of phenolic
compounds being released from the food matrix, thereby pro‑
viding extra hydrogen or electrons to stabilize DPPH radical
by changing them into stable intermediary radicals [38].
The DPPH radical scavenging activityof fresh grape was
found as 3.91 mM Trolox. Most of the raisins have lower
ACs than those of fresh grapes. The drying process may
have destroyed the endogenous antioxidants. However, the
processes may also result in the release or generation of new
compounds which show antioxidant capacity due to the for‑
mation of products of the Maillard reaction or arising from
cell wall impairments [39–41]. According to the findings
of this study, the radical scavenging activity increased in
direct proportion to the rise in temperature (p < 0.05), much
like the results for TPC. AC and TPC should closely corre‑
late. The results of this study support the idea that drying at
high temperatures may promote the release of antioxidants.
It was discovered that the ultrasound-pretreated samples
had lower AC than the untreated samples. Similar to this,
Cruz et al. [26] found that ultrasound application (21.7 kHz,
45 W) decreased the AC (FRAP) of the convectively dried
grape skin due to oxidase activation and cell breakdown.
Higher drying temperatures (40–70 °C) also led to higher
AC. Researchers also discovered that the effect of ultrasound
application is unrelated to temperature, that temperature
application boosts AC and TPC, and that ultrasound applica‑
tion promotes enzyme release and phenolic substance oxida‑
tion by affecting the structure of the cell wall. The TPC and
antiradical activity values of oven-dried grape (Vitislabrusca
L.) pomace gradually increased with drying temperature up
to 80 °C, but further increase (100 °C) resulted in a drop,
according to Demirkol and Tarakci [42].
Phenolic compounds ,such as polyphenols, flavonoids, phe‑
nolic acids, and ascorbic acid (vitamin C) contribute to the AC
of foods [43]. In order to determine the relationship between
VCC and AC and TPC and AC, the correlation graphs were
drawn and given in Fig. 3. It can be stated that both the VCC
and TPC showed a linear relationship with AC except for
VCC and AC of untreated samples (R2 > 0.88). In addition,
it can be concluded that the AC of raisins can be expressed
with VCC and TPC. Also, some vitamins, volatile oils, etc.,
may contribute to AC. Drying air temperature and ultrasound
pretreatment affected the VCC more than the TPC. It is known
that vitamin C can be easily degraded because of oxidation,
heat, light, oxygen, pH, metal ions, etc. [44]. Furthermore,
the sample preparation may be facilitated by the oxidation
and ultrasound application in the 5% ­K2CO3 + 1% OO solu‑
tion may cause the leaching of the VCC into the solution.
Although the change in TPC is small, the high change in VCC
can be explained as the reason for the higher decrease in AC.
Ultrasound applications are generally performed before dry‑
ing to prevent enzymatic and non-enzymatic browning reac‑
tions [45]. Browning levels (A420/g) of ultrasound pretreated
hot air-dried samples are 2.89 (40 °C), 3.36 (50 °C), and 2.80
(60 °C), and unpretreated hot air-dried samples 3.56 (40 °C),
4.38 (50 °C), and 6.35 (60 °C), respectively. It was also deter‑
mined that the browning level of raisins generally increased
with the increase in temperature. In addition, it is expressed that
ultrasound pretreatment reduced the browning levels due to the
limitation of the extent of the Maillard reaction by ultrasound
application [45, 46]. Similarly, Jacob et al. [35] reported that
ultrasound treatment reduced the browning of mature coconut
water. The alcohol soluble color index (A440/g) of ultrasound
pretreated hot air-dried samples are 30.11 (40 °C), 41.16 (50
°C), and 64.95 (60 °C) and unpretreated hot air-dried samples
32.06 (40 °C), 35.75 (50 °C), and 60.57 (60 °C), respectively.
Similar to the results of the browning level, it was deter‑
mined that the soluble color index values in alcohol generally
increased with the increase in temperature.
3.3 Rehydration kinetics of the raisins
One of the quality criteria of the dried product is rehydration
related to microstructural damage. Ultrasound pretreatment
is effective in water recovery of dry foods as it is effective
on mass transfer between solid and liquid surfaces [47]. The
time-dependent water recovery of raisins by rehydration is
given in Fig. 4. According to Fig. 4, it can be said that the
amount of water gainedby the raisins increased with rehy‑
dration time. The high amount of water (around 70%) was
gained in the first 400 min. It may be due to the filling of
capillaries on the surface of the raisins. Free capillaries and
intercellular gaps fill up with water as water absorption pro‑
gresses, which causes the rate of absorption to slow down
[47]. Almost all samples were equilibrated after 800 min.
After 800 min, the weight change of the samples generally
ranged from 0 to 0.01 g. Therefore, the rehydration time can
be considered around 800 min for all samples. Although
the water uptake behavior of the raisin samples was similar
during the rehydration process, the untreated raisins dried
at 40 °C showed the highest water recovery. However, sam‑
ples dried at 50 °C showed the lowest water recovery. It may
be said that excessive drying temperatures and ultrasound
pretreatment may result in higher and irreversible structural
problems [48]. In addition, it was also determined that the
13

Fig. 3  Correlation between
VCC and AC and TPC and AC
of the raisins. a Ultrasound
pretreated samples. b Untreated
samples
rehydration capacity of the ultrasound-pretreated raisins was
lower than the untreated samples. According to Jambrak et al.
[49], although ultrasound pretreatment increased the abil‑
ity of button mushrooms, brussels sprouts, and cauliflower
to retain moisture, increasing the ultrasound intensity (20
to 40 kHz) and application time (3 to 10 min) had a detri‑
mental effect on this ability. The researchers reported that
higher ultrasound intensities cause structural damage and cell
shrinkage. In this study, the rehydration capacity of the rai‑
sins was also adversely affected by ultrasound pretreatment.
Since the ultrasound application damaged the cellular struc‑
ture, the water could not be held in the cell, and therefore the
product may have been less rehydrated.
13
Biomass Conversion and Biorefinery
3.4 Principal component analysis
Principal Component Analysis was conducted on raisin
samples to see whether the samples were grouped differently
according to ultrasound pretreatment and drying air
temperature is given in Fig. 5. In addition, PCA was used
to assess the correlation between the physicochemical
composition of the hot air-dried raisin samples that were
pretreated and unpretreated at various drying temperatures.
For a cumulative variance contribution of 90.15%, the first
variable (F1) accounts for 80.34%, and the second variable
(F2) contributes 9.81% of the variance. The first variable
(F1) is mostly connected with Hue Angle (the highest factor
Biomass Conversion and Biorefinery
Fig. 4  Weight change of the
samples during rehydration time
loadings as 0.983) and the second variable (F2) is mostly
connected with the water activity (the highest factor loadings
as 0.533). According to Fig. 5, the samples are distributed
to all four blocks. F1 was positively correlated with the
40 °C-US-P, 40 °C-NON-P, and 50 °C-NON-P samples,
whereas F1 was negatively correlated with the 50 °C-US-P,
60 °C-US-P, and 60 °C-NON-P samples. On the positive
side of the F1, the samples (40 °C-US-P, 40 °C-NON-P, and
50 °C-NON-P) were related to physical properties and color
values. In addition, it can be stated that physical analysis and
color values (positive side) and chemical analysis (negative
side) were separated by F1. Although the F2 directions for
the samples 40 °C-US-P, 40 °C-NON-P, 60 °C-US-P, and
60 °C-NON-P were all positive, the samples 50°C-US-P and
50 °C-NON-P had a negative correlation. The VVC, TPC,
and AC were strongly correlated with 60 °C-US-P and 60
°C-NON-P samples, whereas the water activity, moisture
content, titratable acidity, L* and HA (°) were strongly
Fig. 5  The results of principal
component analysis
correlated with 40 °C-US-P and 40 °C-NON-P samples.
According to the applied analysis, it can be stated that the
correlations were observed between VVC, TPC, and AC;
RSC, pH, and ΔE; a*, b*, and chroma values; water activity,
moisture content, titratable acidity, L*, and HA (°). The
relationships between VVC and AC and TPC and AC were
also shown in Fig. 3. Chroma was calculated using a* and b*
values. For this reason, this correlation was expected. Water
activity and moisture content values of raisins generally
showed a linear relationship.
4 Conclusion
In this study, the effects of ultrasonic applicationas
pretreatment and drying air temperatures on grape drying
were investigated. This connection examined the effect of
ultrasound pretreatment and drying air temperatures on the
13

drying and rehydration qualities and physicochemical content
of the grapes. The drying time of the samples was shortened
by the increase in temperature and the power of ultrasound
treatment. Thus, it can be concluded that both energy costs
can be reduced and the nutritional value of the products can
be preserved by reducing the exposure time of the products
to hot air. When the chemical composition of raisins was
analyzed, it was found that theVCC was mostly affected by the
ultrasound pretreatment and drying air temperature, then the
RSC, AC, and TPC, in the order (p < 0.05). It was also shown
that an increase in drying temperature resulted in higher
browning, VCC, RSC, TPC, and AC (p < 0.05), as well as
shorter drying time, moisture content, water activity, and color
values. The drying time, moisture content, water activity, and
rehydration capacity of raisins were all considerably reduced
by ultrasound pretreatment (p < 0.05), at the same time
higher values of VCC and TPC were obtained. According
to the results of PCA analysis, for a cumulative variance
contribution of 90.15%, the first variable (F1) accounts for
80.34%, and the second variable (F2) contributes 9.81%
of the variance. The effects of different pretreatments and
drying methods on the quality characteristics of raisins and
the change in quality characteristics of grapes during storage
may be the subject of future studies.
Supplementary Information The online version contains supplemen‑
tary material available at https://d​ oi.o​ rg/1​ 0.1​ 007/s​ 13399-​023-​04269-8.
Author contributions Ahmet Candemir: conceptualization, investiga‑
tion, formal analysis, validation, data curation, writing—original draft.
Gülşah Çalışkan Koç: investigation, formal analysis, methodology,
data curation,writing—original draft.
Safiye Nur Dirim: conceptualization, methodology, data curation,
writing, review and editing.
Ravi Pandiselvam: conceptualization, resources, data curation,
methodology, writing—review and editing.
Data availability All data are available upon request.
Declarations
Ethics approval and consent to participate Not applicable
Consent for publication All authors agreed on the publication of this
research work.
Competing interests The authors declare no competing interests.
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