J Sci Food Agric 2022 Etin

Research Article
Received: 27 April 2022 Revised: 4 August 2022 Accepted article published: 7 August 2022 Published online in Wiley Online Library: 23 August 2022
(wileyonlinelibrary.com) DOI 10.1002/jsfa.12164
Effects of ultrasound pretreatment assisted

drying methods on drying characteristics,
physical and bioactive properties of windfall
apples
Necati Çetin* and Cevdet Sağlam
Abstract
BACKGROUND: Drying is one of the most important post-harvest processes in order to ensure that the products harvested in
certain periods are consumed throughout the year. In this study, Golden Delicious, Oregon Spur and Granny Smith apple cul-
tivars (fallen apples) were dried in open-sun, a controlled glasshouse, microwave oven (200 W), hybrid system (100 W + 60 °
C), convective greenhouse (70 °C) and freeze-dryer (−55 °C) with and without ultrasound pretreatments.
RESULTS: Present findings revealed that the longest drying duration was observed in freeze-drying and the shortest in micro-
wave drying. The greatest color change (ΔE) was observed in ultrasound pretreated Oregon Spur apples dried in a controlled
glasshouse. The greatest total phenolics (40.08 mg GAE g−1), DPPH (2,2-diphenyl-1-picrylhydrazyl) inhibition activity
(46.96%), FRAP (ferric reducing ability of plasma) antioxidant activity (68.01 ∼g Trolox g−1) and ascorbic acid content
(1.52 mg AAE g−1) were observed in open sun-dried Granny Smith apples without ultrasound pretreatment.
CONCLUSIONS: Generally, microwave and hybrid drying yielded better outcomes for bioactive, HMF (5-hydroxymethyl-2-furfu-
ral) and drying characteristics of windfall apples.
© 2022 Society of Chemical Industry.
Keywords: apple; ultrasound; texture; ascorbic acid; phenolic content; color
INTRODUCTION vegetables, poultry, nuts, cereals, etc. are wasted in different

Apple plays a great role in healthy nutrition and is among the most quantities at each stage. Approximately, 30% of fruits and vegeta-
produced and consumed fruit species.1 According to 2019 bles are wasted at the retail and consumption stage, 26% of meat,
poultry, and fish, 15% of nuts, and 41% of sugars and sweet-
data, 87.236.221 tons of apple are produced worldwide from
eners.10 Therefore, drying is among the most suitable method to
4 717 384 ha production lands.2 In terms of annual production quan-
regain these waste fruits. By means of proper drying, waste fruits
tities, China, the United States and Turkey are the leading producers.3
could compete with regular ones in terms of both physical and
Apple is commonly consumed in Western diets.4 Total phenolics
biochemical characteristics.11
(TPs) and ascorbic acid quantity of apples play an important role
Drying is among the oldest methods used for processing and
in sensory quality of fresh and processed fruits.5 Apples are also
preservation of foodstuff. Various physical and chemical changes
known to have health-promoting antioxidant parameters and
are encountered during the process of drying. Such changes des-
have a high antioxidant activity as compared to the other com- ignate sensory and nutritional attributes of the final products.12
monly consumed fruits and vegetables.6 Long-term exposure to high heat levels may result in color loss
Windfall and waste fruits mostly have high moisture contents and significant degradation of heat-sensitive substances. High
and different physical characteristics such as shape, size, color, heat levels may also reduce antioxidant capacity of the dried
and damage levels. Furthermore, they may have greater nutri- products.13 Additionally, new substances are formed through
tional attributes in some cases.7 Long-term exposure to high heat Maillard reaction during the drying process. HMF (5-hydroxy-
levels may result in color loss and significant degradation of heat- methyl-2-furfural) is among these products. HMF is a heat-
sensitive substances. High heat levels may also reduce antioxi-
dant capacity of the dried products.8 Food loss and waste along
the production lines result in different volumes of waste gener- * Correspondence to: N Çetin, Department of Biosystems Engineering, Faculty of
ated at each stage. According to the Food and Agriculture Organi- Agriculture, Erciyes University, 38039, Kayseri, Turkey. E-mail: necaticetin@erciyes.
edu.tr
zation of the United Nations (FAO), food waste is estimated as
413 t at the production stage, 293 t at the postharvest and stor- Department of Biosystems Engineering, Faculty of Agriculture, Erciyes
534
age stage,148 t during the processing.9 Food types such as fruits, University, Kayseri, Turkey
J Sci Food Agric 2023; 103: 534–547 www.soci.org © 2022 Society of Chemical Industry.
10970010, 2023, 2, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/jsfa.12164 by Kaunas University Of, Wiley Online Library on [04/09/2023]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
Evaluation of quality change on dried apples www.soci.org
originated indicator in apple-like products. It is also used as an from the orchards of Yeşilhisar town of Kayseri province in Turkey.
important color indicator to monitor heat treatment during food These apples were collected from 2 m canopy diameter of the
processing.14 trees within 10 days following the harvest season. The apples
Color is an important quality parameter for foodstuff. Color is were then cleaned and sorted into small packets and kept at
also directly related to nutritional attributes of the dried prod- +4 °C until analyses.
ucts.15 Drying processes may result in color changes and nutri-
tional losses. Colored substances play a great role in boosting Drying process
immune system and reduction of degenerative disease risks.16 Initially, windfall apples were collected, and decayed sections were
Ultrasound moves molecules apart as they pass through a liq- removed. They were washed and seeds were removed with the use
uid, while expansion cycles take place when negative pressure is of apple de-seeder. Fresh products then were sliced in 1.4 mm
exerted on the liquid. Cavitation bubbles occur when the dilution cylindrical slices. To determine initial moisture content, 100 g sam-
cycle, which varies depending on the purity and type of ultra- ples were dried in an oven (Memmert UN55; Germany) at 70 °C for
sound liquid with a sufficient level, exceeds the tensile strength.17 24 h in three replicates and average moisture content was deter-
Depending on the system properties, the bubbles continue to mined. Drying process was sustained until an equilibrium moisture.
vibrate at the same frequency as the applied ultrasound. All these Drying methods included open-sun, controlled glasshouse, micro-
effects affect the external resistance and mechanical mixing wave oven (200 W), hybrid system (100 W + 60 °C), air-convective
should affect mass transfer in a similar way.18 The microbubbles dryer (70 °C) and freeze-dryer (−55 °C). For sugar-containing prod-
that occur after cavitation occur at pre-existing weak points in ucts, a drying temperature of 60 to 80 °C is necessary to prevent
the liquid. When cavitation occurs, the growth of sound waves is non-enzymatic browning (Maillard reaction) and to preserve its
due to the absorption of energy from micro gas bubbles irradi- quality.29 Some preliminary tests were performed before the drying
ated with the help of ultrasound. The intensity of the sound experiments started. In addition, some previous apple drying stud-
affects the cavitation, and when a high intensity occurs, cavitation ies were investigated.1,3,30,31
can grow rapidly.19 Ultrasound pretreatments used both during Moisture contents (wet basis, w.b.) were determined with the
the drying process and before to remove moisture from the prod- use of Eqn (1).32
uct positively influence characteristics of final product. For
instance, ultrasound applied during the drying process may W i −W f
Mc = ×100 ð1Þ
improve quality of dried product because of non-thermal nature Wi
of the ultrasounds. Ultrasound could also reduce drying durations
and drying process for heat-resistant substances could be con- where Mc represents moisture content (%, wb), Wi represents the
ducted at lower temperatures.20 initial weight of the product (in grams) and Wf represents the final
In drying process, moisture is removed from the products to weight of the product (in grams).
prevent spoilages encountered in open-sun drying and to pro-
long shelf life. Several new methods have been developed and Open-sun and controlled glasshouse drying
used in industrial drying operations. Although hot-air convective Samples were dried in Kayseri province between the hours 08:00–
drying is the most common and easiest method, low product 18:00 at 25.8–42.5 °C (mean temperature: 25.8 °C) and 48.75% rel-
quality, high energy consumption, color and flavor losses signifi- ative humidity under direct sunlight. Controlled glasshouse has
cantly limit the use of this method. To overcome such deficiencies, the characteristics of: 72 m2 (6 m × 12 m), polycarbonate cover
microwave drying and combined (microwave-assisted convec- (8 mm, 80–85% light transmittance), steel framework, single
tive) drying methods have been developed. These methods offer gable roof, four ventilation and one circulation fans for homoge-
high quality final products, short drying durations and preserved neous air distribution. During the drying process, glasshouse
color, taste and flavor. Despite various advantages, these methods mean temperature was measured as 35.02 °C and relative humid-
may result in fruit browning and taste loss due to excessive heat ity as 34.20%. Glasshouse sidewalls are 4 m high and ridge height
exposure.21-23 Among various drying methods, freze-drying offers is 5 m. Climate parameters (temperature, relative humidity, wind
the best final product quality. However, high operational costs speed and direction) could be arranged with the aid of a control
and relatively longer drying durations are accepted as the most panel equipped with sensors. Sample weights were measured
important disadvantages of freeze-drying. In the literature, there every 2 h in open-sun drying and 1.5 h in controlled glasshouse
are studies in which combined or hybrid drying methods are pre- by using a precise balance (±0.001 g) (Precisa, Sweden). Weighing
ferred in apple drying.6,11,13,24-28 Combination of microwave and was completed in 20 s and samples were replaced into drying
convective drying was used in the majority of these studies. How- environment.33
ever, there are no studies in the literature considering the drying
of windfall apples and ultrasound pretreatment drying processes. Air-convective drying
The aim of this study is to dry windfall apple cultivars with and The air-convective drying experiments were performed in hybrid
without ultrasound pretreatment by different drying methods dryer (Arçelik KMF 833 I; Turkey). In hybrid dryer, microwave and
and to perform a comparative analysis of the determined chro- air-convective characteristics could simultaneously be used.
matic parameters, TP and antioxidant activities, ascorbic acid Ambient temperature could be arranged from 40 to 280 °C. Air-
and HMF contents. convective drying processes were run at 0.5 m s−1 air flow rate
and 70 °C temperature. The oven has a fan for air circulation, per-
forated polyamide platforms and trays to hold the samples. An
MATERIAL AND METHODS AUTOCAD drawing of hybrid dryer is presented in Fig. 1. In
Fresh fruit open-sun drying, apple samples were placed on 50 cm × 50 cm
Windfall apples of Golden Delicious, Oregon Spur and Granny drying papers. Sample weights were measured every 1 h in 70 °
535
Smith cultivars to be used in present experiments were collected C convective oven with the use of a precise balance.25
J Sci Food Agric 2023; 103: 534–547 © 2022 Society of Chemical Industry. wileyonlinelibrary.com/jsfa
www.soci.org N Çetin, C Sağlam
Microwave drying Color measurements

A programmable hybrid dryer (Arçelik KMF 833 I) was used. Micro- Color measurements of fresh and dry products were conducted
waves are released from the upper sections of the oven. The oven with the use of a color measurement device (PCE-CSM 5 PCE
is operated at 2.465 MHz frequency and 900 W output power. The Instruments; Germany). An average of 30 readings was taken for
device operated at 200 W power intensity for different drying every drying treatment. Color measurements were taken from
runs. Microwave drying processes were run at 0.5 m s−1 air flow different points on the surface of dried apple slices. Before each
rate. The drying was performed according to present power and test, device calibration was performed with the use of both black
pre-determined time schedule. Sample weights were measured and white reflector plate. Measurements were performed in CIE-
every 3 min in microwave oven with the use of a precise Lab color space: L* (brightness, 0 dark, 100 bright), a* (+ redness,
balance.25 − greenness) and b* (+ yellowness, − blueness) values were mea-
sured. Measured CIE-L*, a* and b* values were then used to calcu-
Hybrid drying late chroma (C) and total color change (ΔE) values.21 The C and ΔE
Hybrid drying were carried out with the use of hybrid dryer values were determined by the following equations35:
(Arçelik KMF 833 I) with air-convective and microwave character-
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
istics used to dry apple slices. In this hybrid oven, microwave
C = ða*Þ2 + ðb*Þ2 ð2Þ
and convective characteristics could simultaneously be used.
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Hybrid drying processes were run at 0.5 m s−1 air flow rate. The
device operated at 100 W power intensity and 60 °C temperature ΔE = ðL*−L*0 Þ2 + ða*−a*0 Þ2 + ðb*−b*0 Þ2 ð3Þ
for different drying runs. Sample weights were measured every
10 min in hybrid oven by a precise balance.25 where ΔE is the difference between the color of fresh and dried
apple samples; L*0; a*0, and b*0 are the color parameters of fresh
Freeze drying apples; L*, a*, and b* are the color parameters of dried samples.
The laboratory-scale lyophilizator (Teknosem Toros TRS 2/2 V;
Turkey) was used for freeze drying. The lyophilizator is operated Energy consumption
at 10−3 mbar pressure and −55 °C condenser temperature. The Following equations were used to calculate energy consumptions
condenser volume of the lyophilizer used in the study is 5.8 lt, of drying systems.36 A digital watt-meter (Tt Technic PM-001,
and the vacuum pump capacity is 5.4 m3. The device has 2.5 kg Turkey) was used to calculated energy consumption of freeze-
ice production capacity in 24 h. Products were weighed before dryer.
freeze drying and then preserved in a freezer (VWR Symphony
Model 414 005-087; USA) at ultra-low temperature (−80 °C) for E c =Avρ⊍ C ⊍ ΔTt ðgreenhouse and convectiveÞ ð4Þ
24 h.34 E c = ðP +Avρ⊍ C ⊍ ΔT Þt ðhybrid Þ ð5Þ
Ultrasound pretreatment E c =Pt ðmicrowaveÞ ð6Þ
Ultrasound pretreatment was conducted in an ultrasonic bath
(LAB.ULT.4045; Turkey) at 150 W heating power, 40 kHz frequency where Ec is total energy consumption of each drying system
and room temperature (25 °C) for 20 min. Sliced apples were (in kW h), A is cross-sectional area of the plate on which the sam-
placed into a basket, supplemented with distilled water to have ples were placed (in m2), v is air flow rate (in m s−1), ρ⊍ is air den-
a 1:4 distilled water ratio in the ultrasound bath. Ultrasound- sity (in kg m−3), C⊍ is air specific heat capacity (in kJ kg−1 °C), ΔT is
pretreated samples were kept on filter papers for 10 s to remove temperature difference (in °C), t is total drying duration (in hours)
water on surfaces.20 and P is microwave power (in kilowatts).
In the present study, a thermal camera (Testo 872 thermal
imager; Germany, 360 × 240 pixels and ± 0.05 °C) was used to
measure the initial and final temperatures of the samples.
Hardness and fracturability texture profile

Textural properties are critical in determining the acceptance of
dried products; therefore, hardness and fracturability tests of the
dried apples were performed. Hardness and fracturability were
settled as the indexes of texture. These parameters are associated
with large voids in the material and expansion.37 In textural mea-
surements, dried samples were prepared with a radial orientation.
The apple slices were placed on two parallel supports 20 mm
apart, and each support was equipped with a 6-mm-diameter hor-
izontal rod at the tip.38
Hardness and fracturability values of the dried samples were
measured by a texture analyzer (TA.XT Plus; Stable Micro System
Ltd, Godalming, UK) using a 100 kg load cell and a cylindrical
probe (36 mm P/36). Measurement conditions were as follows:
pre-test speed = 2.0 mm s−1; test speed = 2.0 mm s−1; post-test
speed = 10 mm s−1; distance = 2.5 mm. All measurements were
Figure 1. Schematic representation of microwave-convective hybrid replicated three times. In the tests, the hardness (in grams) was
536
dryer. the maximum force required to break the dried sample, and the
wileyonlinelibrary.com/jsfa © 2022 Society of Chemical Industry. J Sci Food Agric 2023; 103: 534–547
fracturability (in millimeters) was the distance at the point of reactive and 2 mL distilled water solution. Resultant mixture was
break; a sample that breaks at a very short distance has a high kept at 25 °C for 3 min, then supplemented with 1 mL sodium car-
fracturability.39 bonate (Na2CO3) solution (Na2CO3 and water, 20:80, g mL−1).
Next, the solution was kept at 20 ± 1 °C for an hour, absorbance
Biochemical analysis readings were performed in a spectrophotometer (UV1800; Shi-
Dry matter, ash and protein content (%) madzu) at 765 nm. Gallic acid standard curves prepared at differ-
Dry matter content was determined through drying samples at ent concentrations were used to determine TP of the samples and
105 °C until a constant mass in an oven (Memmert UN55; results were expressed in milligrams of gallic acid equivalent
Germany). Approximately 1 g of dry sample was ashed in an oven (GAE) per gram of dry apple.41
(Protherm PLF 110; Turkey) at 550 °C for 8 h to determine ash con-
tent. Approximately 0.2 g of sample was used to determine nitro- Total ascorbic acid (TAA) content
gen content with the use of Kjeldahl method. Resultant nitrogen To determine total ascorbic acid (TAA) content, 0.5 mL apple
values were then multiplied by a coefficient of 6.25 to get crude extract was supplemented with 0.5 mL 7.5% trichloroacetic acid,
protein content.40 the resultant mixture was kept at 4 °C for 5 min and filtered (4.5
um). Then, 2 mL of distilled water was supplemented with
Extraction 0.2 mL filtrate and 0.2 mL Folin–Ciocalteu reactive (1:10). Final
Extraction was performed to measure TPs and antioxidant activity solution was kept at room temperature (20 ± 1 °C) in the dark
of dried apples. Before bioactivite analyses, dried apples were for 10 min and absorbance readings were performed in a spectro-
ground using a grinder (Bosch TSM6A014R). For this purpose, photometer (UV1800; Shimadzu) at 760 nm. A calibration curve
3 g of dried apple powder was supplemented into 25 g ethanol generated with the use of known vitamin C concentrations was
(96%). Resultant mixture was processed in an ultrasonic bath used to determine TAA content of the samples and the results
(LAB.ULT.4045) for 15 min. Then, samples were centrifuged at were given as milligrams of ascorbic acid equivalent (AAE) per
1000 rpm for 10 min (Sigma 4-16KS; Germany) and filtered gram of dry apple.41
through 4.5 μm syringe filter. Resultant liquids were stored and
protected from the light. Phenolics and antioxidant properties HMF (5-hydroxymethyl-2-furfural) analysis
were determined.41 HMF (Merck) content of dried apples was determined with the use
of high-pressure liquid chromatography (HPLC; Shimadzu, Tokyo,
Antioxidant capacity Japan) and photodiode array (PDA) detection. Standard HMF solu-
Antioxidant capacity of apple extracts was determined with the tion was prepared in distilled water with the use of chromatogra-
use of the FRAP (ferric reducing ability of plasma) method.42 FRAP phy liquid phase at 95:5 ratio (water and acetonitrile) at HPLC
reactive was prepared through supplementing 2.5 mL purity and standard solution of HMF at different concentration
10 mmol L−1 TPTZ (2,4,6-tri(2-pyridyl)-S-triazine; Merck, Darm- within the range of 6.25 to 50 ppm. Dried apples were ground
stadt, Germany) and 2.5 mL acetate buffer (0.3 mol L−1 pH 3.6) in a laboratory-type grinder and 1 g sample was precisely
into 40 mmol L−1 hydrochloric acid (HCl) and 2.5 mL 20 mmol L−1 (±0.001 g) weighed into 100 mL volumetric flask and dissolved
iron(III) chloride hexahydrate (FeCl3·6H2O) solution. For AC, 30 μL in distilled water. Resultant solution was filtered through
extract and 30 μL distilled water was supplemented with 900 μL 0.45 μm cellulose filter and taken into a vial. Then, 20 μL filtrate
FRAP reactive and the resultant mixture was kept at 37 °C for was injected into HPLC at 1 mL min−1 flow rate and readings were
30 min. Absorbance values were red in a spectrophotometer performed at 285 nm wavelength. Dilution factor and standard
(UV1800; Shimadzu, Kyoto, Japan) at 595 nm. A calibration curve calibration curves were taken into consideration while calculating
was generated with the use ethanol solutions of previously the results. HMF content (in mg kg−1) was calculated in accor-
known Trolox concentrations and results were expressed in milli- dance with the following principle.27
mole Trolox equivalent per gram of dry apple.41
C HMF = ðAN =AC Þ × C 1 × dilution ratio ð8Þ
Antiradical activity
For this purpose, 100 μL samples was mixed with 3000 μL DPPH where AN represents the HMF peak area of experimental solution,
(2,2-diphenyl-1-picrylhydrazyl; Merck) (0.1 mmol L−1 in metha- AC the HMF peak area of standard HMF solution, C1 the concentra-
nol), mixture was vortexed, incubated in the dark for 30 min and tion of standard HMF solution (in mg kg−1) and dilution ratio is
absorbance values were red in an ultraviolet-visible (UV-vis) spec- the sample weight (in milligrams)/experimental samples weight
trophotometer (UV1800; Shimadzu) at 517 nm.43 DPPH radical (in kilograms).
scavenging activity of apple samples was calculated with the
use of the following equation: Experimental design and statistical analysis
In this study, experiments were conducted in randomized blocks
Ac −As split plots experimental design with three replications where a
%Inhibition = ×100 ð7Þ
Ac replicate consisted of ten randomly selected slices from three
apple cultivars to examine the effects of certain independent vari-
where Ac is absorbance of control and As is absorbance of the ables on the dependant responses. Pretreaments (two treat-
extract (sample). ments, control and ultrasound pretreatment) were placed into
main plots and drying methods (six methods) were placed into
Total phenolics (TPs) sub-plots. Each cultivar was statistically evaluated separately.
TPs of apple samples were determined with the use of Folin– The independent variables studied in the full factorial experimen-
Ciocalteu (Merck) method.44 For this purpose, 100 μL apple tal design were cultivar, drying method and pretreatment. The
537
extract was supplemented into 200 μL Folin–Ciocalteu phenol independent variables were chosen in accordance with the
current literature and preliminary tests. The dependent variables was observed in freeze dryer due to longer drying durations, it
investigated were dry matter, ash, protein content, color, texture, was followed by convective drying and the lowest energy con-
HMF and bioactive properties. sumption was seen in open-sun drying. Greater energy consump-
Relationships between drying parameters were determined tions are attributed to longer drying durations and lower energy
with the use of variance analysis (ANOVA). Significant means were consumptions are attributed to greater power outputs. Energy
compared with the use of Tukey's multiple comparison test at consumptions are directly proportional to drying durations. Pre-
95% significance level. The assumptions of normality of error sent findings revealed that microwave drying had lower energy
terms were tested using Kolmogorov–Smirnov and Shapiro–Wilk consumptions than the hybrid drying methods. Such a case was
tests. In addition, skewness and kurtosis values were taken into attributed to the combined energy consumption of both temper-
account for normality. It recommends that a threshold value of ature and microwave power outputs.25
±1.96 for samples less than 50, ±2.58 threshold for samples from
51 to 100, and ± 3.29 for samples larger than 100 should be
Dry matter, ash and protein content (%)
used.45 Since there were 108 samples in the present study, the
threshold value for skewness and kurtosis values was taken Dry matter, ash and protein contents of the cultivars under differ-
as ±3.29. ent drying systems, confidence interval with lower and upper
Homoscedasticity was checked by the Levene test. Together bound, skewness and kurtosis values, the coefficients of determi-
with a homoscedasticity verification, the variance was compared nation (R2, linear) obtained from residual values versus actual
using Tukey's test (homoscedastic distributions). Assumptions of values are provided in Table 2. Dry matter content was found sta-
constant variance were checked by plotting residual versus fits tistically significant (P < 0.05) for Golden Delicious, significant
scatter diagram.46 The scatterplot graph of residuals versus actual (P < 0.01) for Oregon Spur, and insignificant (P > 0.05) for Granny
values allowed noting that the residuals were distributed ran- Smith. Ash values were determined as insignificant (P > 0.05) for
domly around zero with no systematic pattern, satisfying the all cultivars. While the change of the protein content was
assumption of homoscedasticity and zero mean errors. Statistical obtained statistically insignificant for Golden Delicious, and it
analyses were conducted with the use of SPSS version 20.0 was significant (P < 0.01) for Oregon Spur and Granny Smith cul-
software. tivars. In addition, skewness and kurtosis values for dry matter, ash
and protein contents were determined within the limits (±3.29)
suitable for the number of samples (108 samples). The greatest
coefficients of determination was obtained from dry matter con-
RESULTS tent for Granny Smith, and obtained from ash content for Golden
Drying duration and energy consumption Delicious with values of 0.968 and 0.886, respectively. These
Drying duration, final moisture content and energy consumptions values indicate that residuals are close to actual values.
are provided in Table 1. Freeze dryer had the longest drying dura- Significant differences were not observed in control group of
tion, it was followed by open-sun drying and the shortest drying Golden Delicious cultivar. While ultrasound pretreated open sun-
duration was observed in microwave drying system. Freeze dryer dried Golden Delicious apples had the lowest dry matter content
had 180 times longer drying duration than microwave drying. (84.36%), the other treatments were all placed into the same statis-
Ultrasound pretreatments reduced drying durations of all culti- tical group. The greatest ash content (3.19%) was obtained from
vars in hybrid system. Final moisture of apple samples varied the control group of microwave-dried Golden Delicious apples
between 7.41–22.80% (w.b.). Final moistures of ultrasound pre- and the lowest value (2.68%) was obtained from glasshouse-dried
treated cultivars were lower. The greatest energy consumption samples. In ultrasound pretreatment groups, the greatest value
Table 1. Drying time, final moisture content and energy consumption of drying methods
Golden Delicious Oregon Spur Granny Smith
Drying method DT (min) FMC (%) EC (kWh) DT (min) FMC (%) EC (kWh) DT (min) FMC (%) EC (kWh)
Control
Open-sun 1200 16.55 — 1200 17.30 — 960 16.95 —
Glasshouse 720 17.22 12.29 720 18.09 10.13 720 16.95 11.61
Microwave 27 14.90 5.40 24 16.43 4.80 24 16.84 4.80
Hybrid 120 13.68 1.45 130 18.06 2.41 120 13.38 1.73
Convective 480 14.22 15.21 480 14.90 14.07 480 12.25 13.50
Freeze 4320 16.19 30.12 4320 22.80 30.12 4320 14.86 30.12
Ultrasound pretreatment
Open-sun 1200 13.17 — 1080 12.01 — 960 14.03 —
Glasshouse 720 11.37 14.95 720 11.79 13.20 720 14.03 14.08
Microwave 21 10.69 4.20 24 12.31 4.80 24 11.66 4.80
Hybrid 110 11.58 1.69 90 14.90 2.61 110 11.38 2.46
Convective 480 7.42 14.90 480 10.57 13.70 480 9.51 15.15
Freeze 4320 10.20 30.12 4320 10.33 30.12 4320 13.63 30.12
Note: DT, drying time; FMC, final moisture content; EC, energy consumption.
538
Table 2. Dry matter, ash and protein content of dried windfall apples*
Golden Delicious Oregon Spur Granny Smith
Dry Ash Protein Dry Ash Protein Dry Ash Protein

Drying method matter (%) (%) (%) matter (%) (%) (%) matter (%) (%) (%)
Control
Open-sun 91.31a 2.68b 1.89c 88.89b 2.89ab 1.57e 88.29a 2.63c 2.67c
Glasshouse 93.14a 1.68d 2.10b 93.53ab 2.73ab 1.61e 87.91a 2.38c 2.14d
Microwave 92.64a 3.19a 1.73d 94.11ab 3.72ab 2.02c 91.08a 3.16ab 3.44ab
Hybrid 91.85a 1.96cd 1.53e 92.35ab 1.62b 2.55a 85.14a 3.13ab 3.32b
Convective 93.17a 3.02ab 2.55a 94.59a 3.51a 1.82d 88.85a 2.77bc 3.65a
Freeze 92.98a 2.07c 1.82cd 94.42ab 4.02a 2.19b 90.32a 3.27a 3.47ab
Ulltrasound pretreatment
Open-sun 84.36b 2.13bc 2.30d 85.29b 1.69b 2.34c 89.08a 1.05c 3.12b
Glasshouse 91.98a 2.80a 1.77e 91.65a 1.67b 1.98d 89.72a 1.60b 2.38c
Microwave 91.22a 1.49d 3.89a 90.25a 1.68b 2.59b 88.40a 1.64b 3.60a
Hybrid 91.81a 2.16b 2.80c 92.32a 1.83ab 2.99a 86.11a 1.96a 3.03b
Convective 89.35a 1.86c 3.83a 90.99a 1.62b 3.10a 86.24a 1.65b 2.52c
Freeze 91.41a 2.16b 3.10b 94.17a 2.03a 2.19c 87.80a 1.76ab 2.92b
Confidence interval 90.33– 2.09– 2.28– 90.84– 2.14– 2.08– 87.35– 2.00– 2.98–
(95%) 92.20 2.44 3.16 92.92 2.86 2.41 89.14 2.49 3.43
Skewness-kurtosis −1.40– 0.45– 1.53– −0.88– 1.16– 0.38– −0.41– 0.05– 0.59–
2.94 −0.83 1.77 0.43 0.43 −0.75 0.01 −1.29 0.77
F Values 3.071* 0.484 2.045 7.378** 2.252 4.988** 2.179 0.955 24.773**
R2 0.689 0.886 0.563 0.517 0.418 0.497 0.968 0.114 0.712
Mean values with different superscripts in the same column are significantly different; ± SEE, standard error of estimate. *Significant at P < 0.05, **sig-
nificant at P < 0.01. The coefficients of determination (R2, linear) obtained from residual values versus actual values.
(2.13%) was obtained from glasshouse-dried samples and the low- Chromatic parameters
est value (1.49%) was obtained from microwave-dried samples. The The mean L*, a*, b* and ΔE parameters and statistical analysis for
greatest protein content (2.55%) was obtained from convective- Golden Delicious apples are provided in Table 3. The L* values of
dried Golden Delicious apples and the lowest value (1.53%) was control treatments were greater than pretreated samples. How-
obtained from hybrid drying method. In ultrasound pretreatments, ever, a* and b* values were greater in ultrasound pretreated sam-
the greatest value (3.89%) was obtained from microwave drying ples than in the control samples. In all cultivars, the difference of
and the lowest value (2.30%) was obtained from open-sun drying. L* value was statistically significant (P < 0.05) except for Golden
The mean dry matter content of all treatments in control group Delicious cultivar. The change in all other color parameters (a*,
of Oregon Spur cultivar was calculated as 92.98% and the greatest b* and ΔE) were statistically significant (P < 0.01). Additionally,
value (94.59%) was obtained from convective drying. In ultra- skewness and kurtosis values for L*, a*, b* and ΔE were found
sound pretreatments, the lowest dry matter content (85.29%) within the limit values. The highest R2 values were obtained from
was obtained from open-sun drying and the other drying systems a* in Golden Delicious (0.877) and Oregon Spur (0.867), and also
were all placed into the same statistical group. In terms of ash con- determined as 0.933 and 0.905 in b* and ΔE for Oregon Spur,
tents of control groups, the greatest value (4.02%) was obtained respectively.
from freeze drying and the lowest value (1.62%) was obtained In Golden Delicious cultivar, the greatest L* values were respec-
from hybrid drying. In ultrasound pretreatments, ash contents of tively observed in control groups of open-sun, freeze dryer, glass-
the samples varied between 1.36 and 3.87%. In Oregon Spur con- house and hybrid drying methods. The greatest a* value (16.82)
trol group, the greatest protein content was obtained from hybrid was observed in convective drying of ultrasound pretreatment
drying and the lowest value from freeze drying. In ultrasound pre- groups and the greatest b* values were observed in convective
treatment group of Oregon Spur cultivar, the greatest protein (37.76) and hybrid (36.12) drying of the control group samples.
contents were obtained from convective (3.10%) and hybrid dry- The greatest color change (22.91) was observed in convective dry-
ing (2.99%) and the lowest value (1.98%) was obtained from glass- ing of the control group samples.
house drying. Averages for color parameters of Oregon Spur cultivar are pro-
In Granny Smith cultivar, drying methods in both the control vided in Table 4. The greatest brightness (L*) value (74.10) was
and ultrasound pretreatment groups were all placed into the observed in freeze drying of the control groups, the greatest red-
same statistical group. In control groups, the greatest ash content ness (a*,+) value (18.44) was observed in convective drying of
(3.27%) was obtained from freeze drying and the lowest value ultrasound pretreatment groups and the greatest yellowness
(2.38%) from open-sun drying. In ultrasound pretreatment (b*,+) value (42.70) was observed in open-sun drying of ultra-
groups, the greatest value (3.60%) was obtained from microwave sound pretreatment groups. The greatest color change (28.18)
539
drying and the lowest value (2.12%) from open-sun drying. was observed in convective drying of the control groups and
540
wileyonlinelibrary.com/jsfa
Table 3. Chromatic parameters and bioactive properties of Golden Delicious apples under different drying methods
Chromatic parameters Bioactive properties
Antioxidant
Drying Antiradical capacity
methods Pretreatment L* a* b* ΔE TP activity (DPPH) (FRAP) TAA HMF
a ef bc b a c b
Open-sun Control 75.28 ± 1.03 5.21 ± 0.24 25.30 ± 0.94 13.92 ± 1.47 18.69 ± 0.02 32.46 ± 0.65 37.74 ± 2.26 0.78 ± 0.02 18.91 ± 0.95cd
Ultrasound 64.03 ± 3.37bc 7.97 ± 1.93bc 26.95 ± 3.37def 14.44 ± 2.24bc 23.75 ± 0.15a 15.64 ± 1.57d 22.99 ± 0.82ef 0.54 ± 0.01de 3.16 ± 0.16d
Glasshouse Control 74.49 ± 0.98a 7.34 ± 0.60bcd 23.91 ± 0.77f 12.93 ± 0.98c 15.91 ± 0.58c 27.52 ± 0.59b 34.83 ± 1.16c 0.86 ± 0.02a 32.79 ± 1.64c
Ultrasound 58.70 ± 0.42cd 9.64 ± 0.78b 27.54 ± 0.08def 14.19 ± 1.35bc 3.95 ± 0.08e 21.22 ± 0.28c 18.12 ± 0.26g 0.49 ± 0.01ef 8.21 ± 0.41d
Microwave Control 71.18 ± 0.77ab 7.22 ± 1.54bcd 31.06 ± 1.25bcd 15.89 ± 3.17abc 5.78 ± 0.12d 20.93 ± 2.02c 14.24 ± 0.31h 0.63 ± 0.01c 420.38 ± 21.02a
Ultrasound 63.78 ± 6.52bc 5.97 ± 1.06cd 26.62 ± 2.58def 13.10 ± 0.78c 1.98 ± 0.34g 8.58 ± 0.81ef 23.20 ± 1.08ef 0.34 ± 0.01hi 135.94 ± 6.80b
Hybrid Control 74.32 ± 1.71a 5.75 ± 0.81cd 36.12 ± 1.20ab 20.54 ± 3.40ab 2.16 ± 0.11fg 11.04 ± 0.29e 12.85 ± 0.53h 0.45 ± 0.06fg 2.67 ± 0.13d
www.soci.org
Ultrasound 52.61 ± 6.18d 7.97 ± 0.92bc 25.49 ± 1.21ef 15.45 ± 3.16bc 0.69 ± 0.02e 3.67 ± 0.44g 27.25 ± 0.65d 0.30 ± 0.02i 3.33 ± 0.17d
Convective Control 68.47 ± 3.02ab 10.32 ± 0.74b 37.76 ± 1.28a 22.91 ± 2.88a 3.63 ± 0.12e 16.61 ± 0.60d 48.94 ± 2.47a 0.41 ± 0.01gh 4.32 ± 0.22d
Ultrasound 68.03 ± 1.58abc 16.82 ± 0.90a 33.53 ± 0.70abc 20.83 ± 1.13ab 2.12 ± 0.79g 5.64 ± 0.91fg 44.27 ± 1.02b 0.29 ± 0.00i 5.17 ± 0.26d
Freeze Control 75.15 ± 0.91a 4.54 ± 0.57c 29.58 ± 2.24cde 14.45 ± 3.43bc 3.17 ± 0.14ef 23.51 ± 1.88c 25.62 ± 0.59de 0.59 ± 0.05cd 0.12 ± 0.01d
Ultrasound 72.51 ± 3.62ab 5.32 ± 1.64cd 27.67 ± 2.58def 14.05 ± 2.27bc 3.90 ± 0.56e 17.39 ± 0.43d 20.79 ± 0.17fg 0.57 ± 0.02cd 0.22 ± 0.01d

Confidence interval (95%) 65.68–70.75 6.70–8.98 27.75–30.84 14.76–17.36 4.61–9.68 14.13–19.90 23.76–31.38 0.46–0.58 12.87–92.91
Skewness-kurtosis −1.08-0.55 1.56–2.45 0.60 to −0.80 0.92–0.02 1.28–0.08 0.09 to −0.81 0.60 to −0.70 0.48 to −0.61 2.71–6.35
F Values 1.326 13.552** 7.186** 9.674** 35.400** 8.466** 14.806** 6.993** 17.795**
R2 0.533 0.877 0.682 0.827 0.432 0.505 0.970 0.492 0.922
Mean values with different superscripts in the same column are significantly different; ±SEE, standard error of estimate. *Significant at P < 0.05, **significant at P < 0.01. The coefficients of determination
(R2, linear) obtained from residual values versus actual values.
Note: ΔE, total color difference; a, greenness/redness; Antiradical activity (DPPH), DPPH (2,2-diphenyl-1-picrylhydrazyl) inhibition activity (% inhibition); Antioxidant capacity (FRAP), FRAP (ferric reducing
ability of plasma) antioxidant activity (μg Trolox g−1); b, yellowness/blueness; HMF, 5-hidroksimetil-2-furfural (mg kg−1); L, brightness/darkness; TAA, total ascorbic acid (mg AAE g−1); TP, total phenolic (mg
GAE g−1).
J Sci Food Agric 2023; 103: 534–547

N Çetin, C Sağlam
Table 4. Chromatic parameters and bioactive properties of Oregon Spur apples under different drying methods
J Sci Food Agric 2023; 103: 534–547

Antiradical
Drying activity Antioxidant
methods Pretreatment L* a* b* ΔE TP (DPPH) capacity (FRAP) TAA HMF
Evaluation of quality change on dried apples
ab cd abc a-d b c b b
Open-sun Control 67.88 ± 0.83 11.70 ± 0.80 39.74 ± 1.80 21.16 ± 2.77 22.13 ± 0.37 33.60 ± 0.53 40.81 ± 1.68 0.82 ± 0.10 15.43 ± 0.77c
Ultrasound 56.07 ± 6.22cde 15.32 ± 0.28abc 42.70 ± 1.92a 24.93 ± 2.49ab 26.20 ± 0.25a 27.91 ± 0.53d 35.55 ± 0.87c 0.66 ± 0.00cde 7.75 ± 0.39c
Glasshouse Control 68.97 ± 0.79ab 9.65 ± 0.25de 34.59 ± 0.79de 15.82 ± 1.25cde 11.71 ± 0.16c 34.96 ± 1.67c 37.61 ± 1.25c 0.66 ± 0.08cd 3.86 ± 0.19c
Ultrasound 47.01 ± 4.32e 14.72 ± 1.71abc 37.79 ± 3.02bcd 24.97 ± 3.25ab 10.30 ± 0.12d 27.22 ± 1.40d 27.48 ± 0.78d 0.61 ± 0.02de 18.32 ± 0.92c
Microwave Control 55.12 ± 2.03de 13.93 ± 1.26bc 42.34 ± 0.48ab 27.47 ± 2.82ab 9.75 ± 0.17d 38.22 ± 5.38bc 36.42 ± 1.02c 0.95 ± 0.01a 574.01 ± 28.70a
Ultrasound 51.25 ± 5.99e 12.35 ± 0.28cd 38.52 ± 1.27a-d 22.09 ± 3.05a-d 6.89 ± 0.18f 40.23 ± 0.49b 21.07 ± 0.82e 0.76 ± 0.01bc 52.50 ± 2.63b
Hybrid Control 62.68 ± 6.22bcd 13.57 ± 3.53bc 40.45 ± 0.72abc 22.69 ± 4.15abc 10.15 ± 0.16d 20.78 ± 0.54ef 17.27 ± 0.76f 0.81 ± 0.04b 66.76 ± 3.34b
Ultrasound 56.75 ± 1.95cde 15.39 ± 0.68abc 40.02 ± 0.91abc 20.64 ± 0.63bcd 3.98 ± 0.16h 18.68 ± 0.22fg 9.18 ± 0.21g 0.50 ± 0.03ef 6.90 ± 0.35c
Convective Control 55.17 ± 2.41de 16.78 ± 0.26ab 42.35 ± 1.22ab 28.18 ± 1.84a 6.08 ± 0.12g 26.67 ± 0.33d 9.72 ± 0.33g 0.57 ± 0.00de 14.10 ± 0.71c
Ultrasound 54.05 ± 1.77de 18.44 ± 0.61a 40.66 ± 1.22abc 23.27 ± 1.52ab 3.14 ± 0.24i 14.17 ± 0.68g 11.29 ± 0.14g 0.39 ± 0.01f 2.11 ± 0.11c
Freeze Control 74.10 ± 2.95a 5.53 ± 0.67f 36.77 ± 0.77cde 15.13 ± 1.74de 8.15 ± 0.59e 46.26 ± 0.32a 49.72 ± 2.08a 0.73 ± 0.00bc 2.50 ± 0.13c
Ultrasound 66.30 ± 2.21abc 8.50 ± 0.98ef 32.97 ± 2.61e 13.16 ± 2.23e 4.30 ± 0.19h 24.11 ± 1.49de 25.11 ± 0.47d 0.58 ± 0.00de 3.86 ± 0.19c

Skewness-kurtosis 0.12 to −0.74 −0.51 to −0.54 −0.71-0.12 −0.26 to −0.82 1.33–0.79 0.22 to −0.75 0.12 to −1.15 0.10 to −0.42 3.07–8.10
F Values 4.703** 17.399** 10.440** 8.006** 68.739** 9.289** 16.546** 7.687** 6.515**
www.soci.org
R2 0.682 0.867 0.933 0.905 0.352 0.786 0.734 0.536 0.891
GAE g−1).
541
542
Table 5. Chromatic parameters and bioactive properties of Granny Smith apples under different drying methods
Drying Antiradical Antioxidant

methods Pretreatment L* a* b* ΔE TP activity (DPPH) capacity (FRAP) TAA HMF
Open-sun Control 60.76 ± 4.17bcd 16.00 ± 0.77abc 46.10 ± 1.77a 38.37 ± 1.77ab 40.08 ± 0.14a 46.96 ± 1.16a 68.01 ± 0.62a 1.52 ± 0.03a 52.50 ± 2.63c
Ultrasound 46.58 ± 0.82ef 17.88 ± 1.08ab 48.95 ± 0.71a 42.55 ± 1.33a 20.70 ± 0.25b 18.32 ± 0.91e 22.31 ± 0.58h 0.52 ± 0.02f 0.10 ± 0.01e
Glasshouse Control 55.43 ± 2.64de 14.74 ± 0.76abc 41.03 ± 1.83ab 34.99 ± 3.11ab 19.07 ± 0.44b 31.10 ± 0.33cd 38.96 ± 2.34cd 1.08 ± 0.12b 15.67 ± 0.78d
Ultrasound 42.45 ± 3.36f 15.50 ± 1.18abc 37.15 ± 0.65bc 35.05 ± 1.36ab 12.93 ± 0.18c 21.43 ± 0.87e 13.33 ± 2.94i 0.69 ± 0.02de 20.05 ± 1.00d
Microwave Control 69.39 ± 5.45ab 6.99 ± 3.39ef 29.78 ± 7.63cde 19.78 ± 9.76cde 9.33 ± 0.19d 33.69 ± 1.16bcd 13.68 ± 0.23i 0.81 ± 0.00cd 121.18 ± 6.06b
Ultrasound 64.44 ± 5.12abc 11.49 ± 3.56cde 34.61 ± 3.59bcd 23.76 ± 3.99cd 7.77 ± 0.13de 34.81 ± 1.38bc 30.18 ± 2.80fg 0.82 ± 0.01c 132.81 ± 6.64a
Hybrid Control 72.25 ± 2.99a 8.90 ± 2.80def 32.04 ± 3.65cde 21.46 ± 3.92cde 5.96 ± 0.08e 28.36 ± 0.74d 29.94 ± 0.61fg 0.68 ± 0.03de 3.02 ± 0.15e
Ultrasound 58.73 ± 3.02cd 13.08 ± 0.85bcd 33.55 ± 1.31bcd 23.31 ± 2.69cde 6.39 ± 0.10e 39.70 ± 5.56b 54.72 ± 3.02b 0.76 ± 0.04cd 1.63 ± 0.08e
www.soci.org
Convective Control 70.38 ± 3.43ab 11.27 ± 1.40cde 33.41 ± 1.10bcd 23.27 ± 1.02cde 5.94 ± 0.14e 22.27 ± 0.55e 43.22 ± 2.75c 0.62 ± 0.03ef 16.67 ± 0.83d
Ultrasound 66.06 ± 2.74abc 18.83 ± 1.58a 36.86 ± 1.30bc 28.35 ± 1.99bc 3.64 ± 0.26e 18.84 ± 2.51e 25.66 ± 1.64gh 0.49 ± 0.01f 2.03 ± 0.10e
Freeze Control 72.41 ± 2.05a 4.55 ± 1.89f 26.50 ± 2.69de 15.40 ± 2.50de 6.79 ± 2.36e 28.54 ± 2.53d 31.48 ± 0.40ef 0.68 ± 0.06de 15.93 ± 0.80d
Ultrasound 68.64 ± 0.95ab 6.64 ± 0.67ef 23.98 ± 1.08e 12.62 ± 1.25e 5.80 ± 0.18e 29.45 ± 0.43cd 35.88 ± 0.60de 0.72 ± 0.00cde 1.17 ± 0.06e

Skewness-kurtosis −0.77 to −0.42 −0.28 to −1.02 0.19 to −0.59 0.11 to −1.08 1.89–3.04 0.56 to −0.16 0.73–0.14 1.73–2.71 1.55–0.29
F Values 11.766** 13.651** 32.591** 38.641** 27.010** 3.068* 2.400 2.564* 77.655**
R2 0.310 0.538 0.349 0.311 0.346 0.878 0.943 0.575 0.917
GAE g−1).
J Sci Food Agric 2023; 103: 534–547

N Çetin, C Sağlam
the lowest color change (13.16) was observed in freeze drying of (101.67 gf). In the ultrasound assisted group, the greatest values
ultrasound pretreatment groups. were found in the hybrid drying system as 438.98 gf, while
Averages for color parameters of Granny Smith cultivar are pro- open-sun drying, glasshouse, microwave and lyophilizer drying
vided in Table 5. In Granny Smith cultivar, the greatest L* values took place in the same statistical group with the lowest values.
were observed in freeze drying (72.41) and hybrid (72.25) drying The highest hardness values of Oregon Spur cultivar was found
of the control group samples. The lowest L* value (42.45) was in microwave drying with 294.00 gf, and the lowest means was
observed in glasshouse drying of ultrasound pretreatment found in hybrid drying with 98.30 gf. In the ultrasound assisted
groups. While the greatest a* value (18.83) was observed in con- group, glasshouse and hybrid drying systems had the greatest
vective drying of the control groups, open-sun-dried samples hardness values with 475.71 and 442.98 gf, respectively. No dif-
had the greatest b* values (48.95 and 46.10). The greatest color ference was observed in the statistical groupings of the other
change (42.55) was observed in open-sun drying of ultrasound drying methods (P < 0.05). The mean of all drying methods
pretreatment groups. was 390.48 gf in the control group of Granny Smith cultivar,
and this value was the highest mean between cultivar and ultra-
Hardness and fracturability properties sound pretreated. Among the drying methods, the highest
Hardness and fracturability values and statistical groups for vari- value of 885.38 gf was determined in the glasshouse drying.
eties, confidence interval with lower and upper bound, skew- The lowest value was found in the products dried with lyophi-
ness and kurtosis values, the coefficients of determination (R2, lizer. Hybrid and convective drying systems, which had very
linear) obtained from residual values versus actual values are close values of 360.92 and 360.44 gf in the ultrasound assisted
given in Table 6. Hardness values changed as statistically signif- group, respectively. The lowest average was determined in the
icant (P < 0.01) for Golden Delicious, insignificant (P > 0.05) for open-sun drying method.
Oregon Spur, and significant (P < 0.05) for Granny Smith based Fracturability averages were evaluated according to the varie-
on drying methods, while fracturability values were found as ties and pretreatment, the highest average fracturability values
significant (P < 0.01) for Golden Delicious and Granny Smith, of 1.92 mm−1 were obtained in the Oregon Spur ultrasound
insignificant (P > 0.05) for Oregon Spur. Also, skewness and kur- assisted, and the lowest average was 1.29 fracturability mm−1 in
tosis values for fracturability were determined within the limits. the Granny Smith control group. The highest fracturability values
However, these values were obtained for hardness values with- were obtained in the air-convective dried (3.78 fragility mm−1) in
out the limit for Granny Smith (2.15–4.53). Fracturability tests the Golden Delicious control group, and in the glasshouse drying
had high R2 values with the values of 0.995, 0.953 and 0.926 ultrasound group (3.65 fragility mm−1). In Granny Smith cultivar,
for Golden Delicious, Granny Smith and Oregon Spur, the highest values were determined in microwave drying with a
respectively. fracturability of 3.45 and 2.88 mm−1 in both control and ultra-
In the Golden Delicious control groups, the highest hardness sound pretreated groups. No significant difference was found in
values were found in the glasshouse dried (510.19 gf – gram terms of statistical groupings in Oregon Spur untreated and ultra-
force) and the lowest ones was found in the lyophilizer dried sound pretreated groups (P < 0.05).
Table 6. Average values of hardness and fracturability texture profile
Golden delicious Oregon Spur Granny Smith
Fracturability Fracturability Fracturability

Drying method Hardness (gf) (mm−1) Hardness (gf) (mm−1) Hardness (gf) (mm−1)
Control
Open-sun 391.20b 0.85b 144.33bc 0.64a 885.38a 0.86b
Glasshouse 510.19a 2.40ab 226.97abc 1.04a 256.83bc 1.05b
Microwave 168.96cd 1.28b 294.90a 2.65a 294.85bc 3.45a
Hybrid 204.47c 0.82b 98.30c 1.67a 421.91b 0.67b
Convective 453.66ab 3.78a 279.59ab 1.84a 285.34bc 1.07b
Freeze 101.67d 0.46b 142.25bc 0.71a 198.59c 0.63b
Ultrasound pretreatment
Open-sun 241.64b 0.93b 252.15b 2.39a 176.12b 0.58b
Glasshouse 214.94b 3.65a 475.71a 2.54a 248.92ab 1.43ab
Microwave 184.36b 1.02b 228.34b 1.14a 234.06ab 2.88a
Hybrid 438.98a 0.71b 442.98a 2.89a 360.92a 1.55ab
Convective 272.85ab 1.71b 275.40b 2.01a 360.44a 1.72ab
Freeze 111.58b 1.16b 198.66b 0.56a 188.84ab 1.96ab
Confidence interval (95%) 226.61–322.48 1.15–1.98 214.59–295.34 1.29–2.06 259.89–392.14 1.15–1.82
Skewness-kurtosis 0.39 to −1.29 1.38–0.92 0.83–0.16 0.99–0.14 2.15–4.53 0.92–0.32
F Values 5.766** 9.152** 1.959 1.620 2.915* 11.194**
R2 0.853 0.995 0.742 0.926 0.772 0.953
Mean values with different superscripts in the same column are significantly different; ±SEE, standard error of estimate. *Significant at P < 0.05,
**significant at P < 0.01. The coefficients of determination (R2, linear) obtained from residual values versus actual values.
543
Bioactive properties control group samples. The greatest HMF contents were observed
TPs, DPPH, FRAP, TAA and HMF values of Golden Delicious, Oregon in microwave drying of ultrasound pretreatment groups
Spur and Granny Smith cultivars and statistical analysis are provided (132.81 mg kg−1) and microwave drying of the control group
in Tables 3–5, respectively. For Golden Delicious and Oregon Spur samples (121.18 mg kg−1).
cultivars, the change of all bioactive properties were found to be sta-
tistically significant (P < 0.01). However, for Granny Smith cultivar,
the difference of FRAP values were found to be statistically insignif- DISCUSSION
icant (P > 0.05), DPPH and TAA values were significant (P < 0.05), Significant differences were observed in biochemical traits of the
and TP and HMF values were found to be significant (P < 0.01). All cultivars based on pretreatment and drying methods. Biochemi-
skewness and kurtosis values for Golden Delicious were within the cal characteristics of the products largely depend on plant genet-
expected limits, while for Oregon Spur and Granny Smith only the ics, agronomic properties, soil properties and harvest times.48
HMF values were above the expected limits. HMF had the coeffi- Significant losses are encountered in ascorbic acid contents dur-
cients of determination with the values of 0.922, 0.917 and 0.891 ing the drying processes and such losses are not reversed through
for Golden Delicious, Granny Smith and Oregon Spur, respectively. oxidative processes during the rehydration.49 Ascorbic acid is an
In addition, FRAP had the greatest R2 values as 0.970 and 0.943 for essential nutrient. It serves as a biological antioxidant and offers
Golden Delicious and Granny Smith, respectively. protection against diseases.50 High drying temperatures and long
The greatest TPs were observed in sun-dried samples and the drying durations may degrade phenolic compounds and reduce
lowest in hybrid drying of ultrasound pretreatment groups antioxidant activity.51 Similar effects were reported during the
(0.69 mg GAE g−1). Free radical DPPH antioxidant is among the drying processes of Aronia fruits.52 However, Igual et al.53
most commonly used compounds to determine radical scaveng- reported that dry apricots had greater antioxidant activity than
ing activities.47 In Golden Delicious apples, the greatest DPPH% the fresh ones. Such a case may be related to greater antioxidant
inhibition value was observed in open-sun drying of the control capacity of partially oxidized polyphenols than non-oxidized poly-
group samples, followed by glasshouse drying of the control phenols54 and formation of new compounds like Maillard reaction
groups. The lowest value was observed in hybrid drying of the products.
ultrasound pretreatment groups. For FRAP activity of Golden Deli- Drying can degrade bioactive components in fruits due to high
cious apples, the greatest value (48.94 μg Trolox g−1) was temperatures and long drying times.55 Ultrasound pretreatment
observed in convective drying of the control group samples and is one of the best way to preserve nutrients during drying. It has
the lowest value (12.85 μg Trolox g−1) was observed in hybrid been determined that pretreatment preserves the natural flavor,
drying of the control groups. The greatest ascorbic acid content color and heat-sensitive nutritive components of the fruits and
(0.86 mg AAE g−1) was observed in glasshouse drying of the con- reduces the drying time. Additionally, because of ultrasounds
trol group samples and the lowest values were observed in con- use of liquid media, the transport of solutes or liquids promotes
vective (0.29 mg AAE g−1) and hybrid (0.30 mg AAE g−1) drying nutrient loss, especially soluble nutrients.12 Opalić et al.12 indi-
of the control group samples. The greatest HMF content cated that prolonged ultrasound pretreatment resulted in a
(420.38 mg kg−1) was observed in microwave drying of the con- reduction in total phenols and flavonoids, as well as the antioxi-
trol group samples. dant capacity of dried apples. In addition, the authors reported
TPs, DPPH, FRAP, TAA and HMF values of Oregon Spur apples are that sugar content and bioactive compounds decreased in apple
provided in Table 4. In Oregon Spur cultivar, the greatest TPs samples subjected to long ultrasound pretreatment. TP content
(26.20 mg GAE g−1) were observed in open-sun drying of the con- was greater in dried apple than in fresh samples. However, lon-
trol group samples and the lowest value (3.14 mg GAE g−1) in con- gest ultrasound pretreatment had lower TP as 3.38 mg g−1, while
vective drying of ultrasound pretreatment groups. The greatest the shortest pretreated samples had the highest TP with the value
DPPH% inhibition (46.26%) was observed in freeze drying of the of 5.47 mg g−1.12
control group samples and the lowest (14.17%) in convective dry- In another study, it has been reported that an increase in A, B
ing of ultrasound pretreatment groups. The greatest FRAP activity and E vitamin content can be observed after drying, but this effect
(49.72 μg Trolox g−1) was observed in freeze drying of the control tends to have a dual effect at the highest temperatures tested
group samples and the lowest values were observed in convective with ultrasound pretreatment.56 Rodríguez et al.14 reported that
drying (9.18 μg Trolox g−1) of the control groups and hybrid drying ultrasound-assisted drying of apple cubes also contributed to
(9.72 μg Trolox g−1) of ultrasound pretreatment groups. The great- the reduction of quality loss of apple cubes regarding polyphenol
est ascorbic acid content (0.95 mg AAE g−1) was observed in content, flavonoid content, and antioxidant activity.
microwave drying of the control group samples and the lowest In general, microwave-dried products had greater antioxidant
(0.50 mg AAE g−1) in hybrid drying of ultrasound pretreatment (DPPH) activity than the convective-dried products. Such a case
groups. The greatest HMF content (574.01 mg kg−1) was observed was attributed to shorter drying durations and free radical scav-
in microwave drying of the control group samples. enging activity of Maillard reaction products.53 Additionally,
TPs, DPPH, FRAP, TAA and HMF values of Granny Smith apples increasing drying temperatures and microwave powers might
are provided in Table 5. The greatest TPs (40.08 mg GAE g−1) have reduced TPs and antioxidant activity. Longer drying dura-
were observed in open-sun drying of the control group samples. tions may result in oxidation and degradation of phytochemicals
The greatest DPPH antioxidant activity (46.96%) and the greatest with a high antioxidant potential54 and loss of bioactive proper-
FRAP (68.01 μg Trolox g−1) were also observed in open-sun dry- ties.36 Enzymatic and non-enzymatic browning reactions encoun-
ing of the control group samples. The lowest FRAP values were tered during the drying process may also influence antioxidant
observed in glasshouse drying of ultrasound pretreatment groups characteristics.52
(13.33 μg Trolox g−1) and hybrid drying of the control group sam- In the present study, this effect was observed in two of three
ples (13.68 μg Trolox g−1). The greatest ascorbic acid content apple cultivars, but not observed in Granny Smith cultivar. This
544
(1.52 mg AAE g−1) was observed in open-sun drying of the phenomenon can occur in two directions, depending on the
species and cultivars. In some apple cultivars, freeze drying for 70 °C oven drying and as 61.88 and 38.52% for 180 W micro-
increased porosity, then increased antioxidant (DPPH) activity. wave drying power. Rodríguez et al.14 reported antioxidant
Thus, high phenolic levels of freeze drying could be related to (FRAP) activity of Granny Smith apples without ultrasound pre-
such increasing efficiencies.57 Similar findings were also indicated treatment, with ultrasound-1 (18.5 kW m−3) and ultrasound-2
by Atalay and Erge58 for the mushroom dried with the use of (30.8 kw m−3) treatments respectively 51.2, 49.3 and 37.8 mg g−1
hybrid drying. The researchers reported that the antioxidant activ- for 30 °C drying temperature, as 45.6, 40.4 and 39.6 mg g−1 for
ity of the samples significantly increased with the increment 50 °C drying temperature and as 38.1, 39.7 and 41.6 mg g−1 for
of microwave power from 90 to 600 W. Authors also attributed 70 °C drying temperature. Similar with the present findings,
this increase to the release of TPs from the tissues by the deterio- Kaya27 reported HMF content of Starking Delicious apples as
ration of the cell wall structure due to the intense heat by pro- 18.52 mg kg−1 for 65 °C drying temperature, 6.27 mg kg−1 for
duced microwave. The higher polyphenol content in some of 15 min ultrasound pretreatment and as 5.41 mg kg−1 for 30 min
the dried apples than in fresh apples may be due to the presence ultrasound pretreatment. HMF value was reported as
of other antioxidant substances produced during drying and 312.69 mg kg−1 for 180 W microwave power, as 279.05 mg kg−1
reacting with the Folin–Ciocalteu reagent.59 In addition, ultra- for 15 min ultrasound pretreatment and as 189.53 mg kg−1 for
sound pretreatment of apples shortens the drying time with 30 min ultrasound pretreatment.
dehumidified air, reducing product exposure to hot air and oxy- The textural properties of dried samples depend on the behav-
gen. In this case, it probably contributed to the greater retention ior of the soluble solid phase and cellular matrix in the tissue, by
of the polyphenols. In addition, tissue damage caused by ultra- different interactions with water. In air-convective drying, the sur-
sound and high temperature can lead to increased extractivity face moisture is quickly remowed, hardness is described by the
of polyphenols.60 curing phenomenon, thus forming a harder outer layer on the
In the present study, the lowest HMF contents were observed in fruit. Additionally, the amount and composition of pectin can
freeze drying and the greatest in microwave drying. As compared affect the structure and textural properties of air-dried apple tis-
to the other drying methods, microwave might have induced sues.62 Similar to the present study, Mothibe et al.62 evaluated
HMF formation. In general, ultrasound pretreated samples and the hardness values for dried apples for different drying condi-
longer drying durations yielded lower HMF values. Therefore, it tions. The hardness values were found to be 1533.102 gf for fluid
could be stated that ultrasound pretreatments reduced HMF con- bed dryer (70 °C). In addition, it was determined as 555.485 gf for
tents. Dried products generally have greater protein ratios due to 5 min pretreatment, 592.926 gf for 10 min pretreatment, 508.078
water loss encountered during the process of drying. Similar with gf for 15 min pretreatment for the products dried in fluid bed
the present findings, Polat et al.26 reported the greatest protein dryer with ultrasound pretreatment applied. Khampakool et al.63
content (2.5%) of apples in hybrid drying (microwave + vacuum) determined the hardness values for dried bananas as 7.9 N and
for 30 min at 300 W to 400 mmHg drying conditions. Researchers fracturability values as 1.6 mm−1 for freeze-drying. In three differ-
also reported L* values of different drying methods as between ent microwave applications of Duan et al.64 dried sweet potato,
53.23 and 78.27. It has been reported that exposure to ultrasonic the hardness and fracturability values were approximately 4 N
waves tends to decrease L* values. Since the ultrasound destruc- and 1.7 mm−1 for 0.125 W g−1 application, 7.2 N and 1.5 mm−1
tion of the cells releases enzymes responsible for the browning for 0.225 W g−1 application and 8.0 N and 1.75 mm−1 for
of the surface, which leads to the dark color. However, there is 0.370 W g−1 application, respectively.
no no clear trend for either a* or b* values for all dried apple
samples.61
Complying with the present findings, Vega-Gálvez et al.6 CONCLUSION
reported DPPH values of dried Granny Smith apples at 0.5 m s−1 In the present study, windfall apples of Golden Delicious, Oregon
air flow rate and 40, 60 and 80 °C drying temperatures respec- Spur and Granny Smith cultivars were dried without and with
tively as 1787.99, 3113.47 and 2142.96 μg mg−1, TPs respectively 20 min ultrasound pretreatment in open-sun (0.5 m s−1 air flow
as 31.94, 27.39 and 27.34 mg GAE 100 g−1, ΔE color change rate), controlled glasshouse, microwave (200 W), hybrid (100 W
values as 35.70, 28.15 and 18.75. Masztalerz et al.28 dried apples + 60 °C), convective (70 °C) and freeze dryer. Initial moisture con-
with the use of osmotic dehydration pretreatments and different tent of Golden Delicious, Oregon Spur and Granny Smith apples
drying methods and reported FRAP values as between 1.96 and was respectively measured as 85.22, 83.45 and 80.02% and final
14.23 mmol trolox 100 g−1 dm. Opalić et al.12 applied different moisture contents varied between 7.42–22.80% (w.b.). Present
ultrasound pretreatment durations and reported the lowest TPs findings revealed that ultrasound pretreatments reduced drying
(3.38 mg g−1 s) for 54 min ultrasound pretreatment and 540 min durations. For color parameters, control samples of all cultivars
convective drying (71.5 °C) and the greatest (5.47 mg g−1) for had greater L* values, but ultrasound pretreated samples had
22.5 min ultrasound pretreatment and 720 min convective greater a* values. The greatest color change was observed in con-
(71.5 °C) drying. The lowest FRAP value (2.5 mmol L−1 Fe(II) g−1) vective drying of Golden Delicious and Oregon Spur cultivars and
was reported for 54 min ultrasound pretreatment and 540 min open-sun drying of Granny Smith cultivar. The greatest energy
convective (71.5 °C) drying and the greatest (4.0 mmol L−1 consumption was observed in freeze dryer and the lowest in
Fe(II) g−1) for 22.5 min ultrasound pretreatment and 720 min con- hybrid dryer. Bioactive properties values were generally greater
vective (71.5 °C) drying. Horuz25 dried Golden Delicious apples in control group samples of all cultivars. Considering the entire
with convective drying at 50, 60 and 70 °C temperatures and cultivars and drying systems together, the greatest TPs was
reported antioxidant capacity (DPPH, % inhibition) respectively observed in open-sun drying and the greatest HMF values were
as 28.29, 25.53 and 25.40%. Antioxidant activity (DPPH, % inhibi- observed in microwave drying. Color, biochemical traits and dry-
tion) was reported as 25.62% for hybrid drying (120 W + 60 °C). ing characteristics of windfall and regular apples were generally
Al Juhaimi et al.24 reported antioxidant activity of Granny Smith similar with the literature findings. Significant positive effects
545
and Golden Delicious apples respectively as 52.49 and 34.04% were observed in terms of protein content, color characteristics
and drying times in ultrasound pretreated products. Ultrasound 16 Cetin N, Yaman M, Karaman K and Demir B, Determination of some
pretreatment is recommended to improve these properties. How- physicomechanical and biochemical parameters of hazelnut (Cory-
lus avellana L.) cultivars. Turk J Agric For 44:439–450 (2020).
ever, no significant difference was found in terms of bioactive 17 Çiçekdağı F, Influential Parameters on Acoustical Cavitation Which is
properties and HMF content. Created by Ultrasonic Waves and Measuring Cavitation Energy. Istan-
bul Technical University, Graduate School of Natural and Applied
Sciences, Master Thesis, Istanbul, p. 101 (In Turkish) (2011).
DISCLOSURE STATEMENT 18 Leighton TG, The principles of cavitation, in Ultrasound in Food Proces-
sing, Vol. 12. Blackie Academic & Professional, an Imprint of Thom-
The authors report no conflicts of interest. The authors alone are
son Science, London, UK (1998).
responsible for the content and writing of the article. 19 Maynard JD, Innovative Acoustic Techniques for Studying New Materials
and New Developments in Condensed Matter Physics. Pennsylvania
State University Park Department of Physics, Pennsylvania, USA
ACKNOWLEDGEMENTS (2000).
This study was derived from PhD Thesis of Dr Necati Çetin at 20 Nowacka M, Wiktor A, Śledź M, Jurek N and Witrowa-Rajchert D, Drying
of ultrasound pretreated apple and its selected physical properties.
Department of Biosystems Engineering, Graduate School of Natu- J Food Eng 113:427–433 (2012).
ral Sciences, Erciyes University, Kayseri, Turkey. The authors would 21 Zia MP and Alibas I, The effect of different drying techniques on color
like to express their gratitude to Assoc. Prof. Dr Kevser Karaman, parameters, ascorbic acid content, anthocyanin and antioxidant
Prof. Dr Mahmut Kaplan and Beyza Çiftçi for their support of the capacities of cornelian cherry. Food Chem 364:130358 (2021).
22 Zielinska M and Michalska A, Microwave-assisted drying of blueberry
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(Vaccinium corymbosum L.) fruits: drying kinetics, polyphenols,
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FBA-2020-10157). 212:671–680 (2016).
23 Pinar H, Çetin N, Ciftci B, Karaman K and Kaplan M, Biochemical compo-
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Research Article

(wileyonlinelibrary.com) DOI 10.1002/jsfa.12164

Effects of ultrasound pretreatment assisted

Keywords: apple; ultrasound; texture; ascorbic acid; phenolic content; color

INTRODUCTION vegetables, poultry, nuts, cereals, etc. are wasted in different

Microwave drying Color measurements

Hardness and fracturability texture proﬁle

Golden Delicious Oregon Spur Granny Smith

Golden Delicious Oregon Spur Granny Smith

Dry Ash Protein Dry Ash Protein Dry Ash Protein

Chromatic parameters Bioactive properties

© 2022 Society of Chemical Industry.

J Sci Food Agric 2023; 103: 534–547

J Sci Food Agric 2023; 103: 534–547

© 2022 Society of Chemical Industry.

R2 0.682 0.867 0.933 0.905 0.352 0.786 0.734 0.536 0.891

Chromatic parameters Bioactive properties

Drying Antiradical Antioxidant

© 2022 Society of Chemical Industry.

J Sci Food Agric 2023; 103: 534–547

Table 6. Average values of hardness and fracturability texture proﬁle

Golden delicious Oregon Spur Granny Smith

Fracturability Fracturability Fracturability

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