Journal of Food Engineering 369 (2024) 111944

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Journal of Food Engineering

journal homepage: www.elsevier.com/locate/jfoodeng

Effects of different pre-freezing methods and pressure levels on the pore

structure and mechanical properties of microwave-vacuum dried apple
Yasumasa Ando *, Daisuke Nei
Institute of Food Research, NARO, 2-1-12 Kannondai, Tsukuba, Ibaraki, 305-8642, Japan

A R T I C L E I N F O A B S T R A C T

Keywords: The present study describes the effects of different pre-freezing methods with microwave-vacuum drying (MVD)
Microwave-vacuum drying at different pressure conditions (no vacuum or at 1, 3, or 8 kPa) on the three-dimensional pore structure and
Pre-freezing mechanical properties of dried apples. Slow-freezing pretreatment and lower pressure conditions were shown to
Apple
be effective in reducing the drying time in MVD. Slow-frozen MVD samples had large pore sizes and high
X-ray computed tomography
Three-dimensional pore structure
porosity, especially the mean pore equivalent radii of the slow-frozen MVD samples at 1 and 3 kPa were 153.7
Mechanical properties and 138.7 μm, which are comparable to that of the freeze-dried sample (137.7 μm). These structural charac­
teristics were thought to confer low hardness and high crispness in the samples. Principal component analysis
revealed that the structural properties of the pores in MVD samples were decided not by the pressure condition,
but by the pre-freezing method. Overall, the results showed that the combination of slow-freezing pretreatment
with MVD under a lower pressure is advantageous for improving the drying efficiency and the texture of the
dried samples. The slow-frozen MVD samples were structurally similar to the freeze-dried samples, but there
were some differences in the mechanical properties, suggesting that there are factors other than the pore
structure that influence the mechanical properties.

1. Introduction
The global market for processed fruits and vegetables, including
those that are fresh, canned, fresh-cut, frozen, dried and/or dehydrated,
has grown with the recent increases in the health consciousness of
consumers and the demand for convenient products that help save time
and effort. The market size was valued at more than USD 320 billion in
2022, and it is expected to grow with a compound annual growth rate of
over 5.5% from 2023 to 2032 (Global Market Insights, 2022). Among
processed fruits and vegetables, dried fruits are consumed worldwide as
a shelf-stable and palatable snack, and as a good source of nutrients,
such as vitamins, minerals, fiber, and phytochemicals. In the production
of dried fruits, raw materials have generally been processed by
sun-drying or industrial air-drying (AD), but some high-quality dried
products that are processed by costly methods, such as freeze-drying
(FD) and microwave-drying, are also available on the market.
Microwave-vacuum drying (MVD) is a relatively new drying tech­
nique that has been applied to many fruits and vegetables (Reis et al.,
2022). Under microwave irradiation, heat is generated within the
product through the excitation of water molecules, which promotes
moisture transfer inside the product (Datta and Rakesh, 2013). Since the
boiling point of water decreases at lower pressures, the supplied mi­
crowave energy is efficiently consumed by water evaporation. Due to
this mechanism of water transfer, MVD has the advantages of a high
drying rate and suppression of excessive increases in the sample tem­
perature, which usually lead to quality deterioration (Zhang et al.,
2006). To date, there have been many reports on the use of MVD in
drying fruit, such as kiwifruits (Tian et al., 2015), apples (Ando et al.,
2019a), cranberries (Zielinska et al., 2017), and tomatoes (Durance and
Wang, 2002; Orikasa et al., 2018). These studies have shown the ad­
vantages of MVD, including the high drying rate (Zielinska et al., 2017),
high energy efficiency (Durance and Wang, 2002), less change in the
surface color (Tian et al., 2015), and high retention of nutrients and
antioxidant activity (Orikasa et al., 2018). Although FD can produce
high-quality dried products with less shrinkage and higher retention of
nutritional value and color compared to AD and MVD (Lin et al., 1998),
MVD has a great advantage of having by far the shortest drying time (Lin
et al., 1998; Ando and Nei, 2023).
In recent years, fundamental studies such as analyses of moisture
distribution using hyperspectral imaging during MVD (Ren and Sun,
2022; Pu and Sun, 2015) and shrinkage phenomena by in-situ and

* Corresponding author.
E-mail address: yaando@affrc.go.jp (Y. Ando).

https://doi.org/10.1016/j.jfoodeng.2024.111944
Received 17 October 2023; Received in revised form 19 December 2023; Accepted 5 January 2024
Available online 11 January 2024
0260-8774/© 2024 Elsevier Ltd. All rights reserved.
Y. Ando and D. Nei
Nomenclature
AD air-drying
CT computed tomography
FD freeze-drying
MVD microwave-vacuum drying
NV no vacuum
PCA principal component analysis
ROI region of interest
continuous measurements of mass and shape (Ishibashi et al., 2022)
have been performed. In addition, applied technologies are being
developed, such as temperature control through output manipulation
(Ando and Okada, 2023; Bórquez et al., 2015) and the continuous flow
MVD system at the industrial level (González-Cavieres et al., 2021), with
the aim of improving productivity and obtaining high-quality dried
products. However, in some cases, hardening associated with the severe
deformation and shrinkage of dried products can occur due to rapid
water evaporation within the tissue during MVD (Ando et al., 2019a;
Chong et al., 2014).
For the drying of fruits and vegetables, it has been reported that
pretreatment, such as thermal blanching (Cheng et al., 2015), ultra­
sound (Huang et al., 2020), freezing (Ando et al., 2019c), pulsed electric
field (Ade-Omowaye et al., 2001), or high hydrostatic pressure treat­
ment (Santos et al., 2022), is effective for enhancing the drying process
and improving the quality of the dried products (Deng et al., 2019;
Lewicki, 1998). Of these pretreatment methods, freezing is the most
effective method for increasing the drying rate (Ando et al., 2016;
Dandamrongrak et al., 2002) and preventing sample deformation (Ando
et al., 2019b; Tatemoto et al., 2016). Our previous study showed that
pre-freezing increased the drying rate by approximately 1.2–1.3 times in
the MVD of apple, and reduced the pressure difference between the in­
side and outside of the sample tissue, which is the cause of the shrinkage,
resulting in porous dried products with high crispness (Ando et al.,
2019a).
However, these results were obtained using a single pre-freezing
condition with a single pressure condition for MVD, and the effects of
different freezing rates and pressure levels in MVD on shrinkage and the
mechanical properties of the dried products remain unknown. Clarifi­
cation of these issues may contribute to our accumulating knowledge,
and facilitate the optimization of MVD with pre-freezing. In the present
study, apple, which is a popular fruit that is often consumed as a dried
product, was pretreated by freezing at different freezing rates, and dried
by MVD under different pressure conditions. Subsequently, the three-
dimensional pore structure and mechanical properties of the dried
samples were investigated, and principal component analysis was per­
formed on the parameters extracted for both the pore structure and
mechanical properties to characterize the quality attributes of the ob­
tained dried samples.
2. Materials and methods
2.1. Sample preparation
Apples (Malus pumila var. domestica) of the Fuji cultivar were ob­
tained from a local market, and stored in a refrigerator at 5 ◦ C until used
for the experiments. For the following drying experiments, apples were
peeled and cored with a cork borer, and the flesh was cut into a quarter
circle (approximately 30 mm radius and 10 mm thickness) circle with a
sharp knife; these slices were used as the tissue samples. The samples
were subsequently frozen by slow-freezing or rapid-freezing before
drying. For slow-freezing, the samples were placed on a polystyrene
foam board, and frozen in static air overnight in a freezer (SC-DF25K,
2
Journal of Food Engineering 369 (2024) 111944
Nihon Freezer Co., Ltd., Tokyo, Japan) set at − 20 ◦ C. For rapid-freezing,
the samples were frozen in an air-blast freezer (FMF-038F1, Fukushima
Industries Corp., Osaka, Japan) set at − 40 ◦ C for 40 min. All frozen
samples were then wrapped in cling film, and stored in a chest freezer
(SF–3120F3; Nihon Freezer Co., Ltd.) at − 40 ◦ C until used for the ex­
periments. The frozen samples were thawed in an incubator at 25 ◦ C for
3 h before being used as pre-frozen samples.
The initial moisture content of the fresh samples was gravimetrically
determined according to the standard method used in the previous study
(Ando and Okada, 2023). Briefly, a fresh sample was milled and mixed
with a drying aid (Celite No. 503; Imerys Filtration Minerals Inc., San
Jose, CA, USA). The mixture in an aluminum cup was placed on a hot
water bath set to 70 ◦ C to pre-dry the mixture until it became powdery.
Then, the mixture was completely dried in a vacuum drying oven
(AVO-250NS; AS ONE Co., Osaka, Japan) at 70 ◦ C until the mass of the
mixture reached an equilibrium. The initial moisture content was
determined to be 5.322 ± 0.016 on a dry basis (g-water/g-dry) from the
average of eight samples.
2.2. Drying procedure
In the MVD experiment, a glass desiccator containing eight samples
(42.6 ± 2.6 g-fresh weight) was placed in a microwave reactor (μReactor
Ex; Shikoku Instrumentation Co., Ltd., Kagawa, Japan). The reactor
cavity (internal size: 280 mm in width, 250 mm in height, and 280 mm
in depth) was connected to a microwave generator with a maximum
output power of 1 kW at 2450 MHz. The inside of the desiccator was
depressurized using a vacuum pump (G-50DA; Ulvac Kiko Inc., Miya­
zaki, Japan). To evaluate the effects of the pressure level on the drying
characteristics, MVD was performed under atmospheric pressure (no
vacuum; NV) or reduced pressure conditions. In the study of MVD of
fruits and vegetables, the pressure around 1–10 kPa is often used,
therefore, for drying under reduced pressure, the internal pressure was
maintained at 8, 3, or 1 kPa throughout the drying process using a
pressure regulation unit (NVC–2300B; Tokyo Rikakikai Co., Ltd., Tokyo,
Japan). For MVD under NV, drying was carried out without the
connection of a vacuum hose.
The samples were irradiated with microwaves at an output power of
200 W (4.7 W/g-fresh weight) with 5-s irradiation/5-s pause cycles,
which have been determined to prevent excessive increases in the
sample temperature. After the specified drying times, the samples were
removed from the apparatus, and weighed to calculate the moisture
content. Samples were dried until the moisture content reached below
0.20 on a dry basis (g-water/g-dry), then subjected to AD at 60 ◦ C to
remove any residual moisture to equalize the moisture condition for the
subsequent X-ray computed tomography (CT) and mechanical tests. AD
and FD were employed for the comparison of the quality attributes of the
dried samples. AD samples were obtained by drying the samples in a
drying chamber (SM4S-EH, Kihara Works Co., Ltd., Yamaguchi, Japan)
at 60 ◦ C; the air velocity in the chamber was 0.26 m/s. For FD, the frozen
samples were dried in a manifold freeze dryer (FD-4-U; Nihon Techno
Service Co., Ltd., Ibaraki, Japan). After the frozen samples were placed
in the drying bottles, the inside of the bottles was depressurized by a
vacuum pump. The drying proceeded at a controlled room temperature
of 25 ◦ C and the pressure was maintained at less than 10 Pa during
drying. Only slow-freezing was applied as a pre-freezing for FD, because
rapid-frozen samples form cracks during the drying that affect the
analysis of pore structure.
2.3. X-ray computed tomography
The internal pore structure of the dried samples was evaluated using
an X-ray CT system (SMX-100CT; Shimadzu Corp., Kyoto, Japan). A
small block (approximately 3 mm × 3 mm × 6 mm) was cut from the
central part of the dried sample with a sharp knife, then scanned at an X-
ray tube voltage of 100 kV and a current of 40 μA. The 600 transmission
Y. Ando and D. Nei Journal of Food Engineering 369 (2024) 111944

images were obtained through 360 degrees of rotation with a voxel 3. Results and discussion
resolution of 5.2 μm. The obtained raw grayscale images were processed
using Amira 3D software 2022.2 (Thermo Fisher Scientific Inc., Wal­ Fig. 2 shows the changes in the moisture content during MVD. In the
tham, MA, USA) to analyze the pore structure of the dried samples. Fig. 1 non-frozen MVD samples, the drying time was 140 min under atmo­
shows the overall flow of the image-processing procedures. The region spheric pressure, and 130, 100, and 90 min under reduced pressure at 8,
of interest (ROI) was cropped to a size of 320 × 320 × 500 voxels 3, and 1 kPa, respectively, indicating that the drying time was shortened
equivalent to 1664 × 1664 × 2603 μm3 from the central part of each by the lower pressure conditions (Fig. 2a). This trend was consistent
image to avoid artifacts on the sample edges (Fig. 1a). The images were with that of the study by Kurata et al. (2020) who reported shorter
denoised in three-dimensional space with a non-local means filter, then
binarized using an interactive thresholding module (Fig. 1b). Subse­
quently, the individual pores were segmented (Fig. 1c). Individual three-
dimensional objects with less than 100 voxels were considered to be
noise, and were removed. To facilitate quantitative analysis, the pores
intersecting the boundaries of the ROI were removed to exclude the
pores with improper structures. After the segmentation, a pore network
model was generated using a pore network modeling module to evaluate
the structural characteristics and connectivity of the pores inside the
dried samples. The equivalent radius of the pore and channel length and
the equivalent radius of throats connected to each pore were determined
as indicators of pore connectivity. Porosity was defined as the ratio of
the total pore volume to the ROI volume. Scans were performed for three
samples from each condition.

2.4. Mechanical properties

The puncture test was used to evaluate the mechanical properties of

the dried samples according to the procedure described in our previous
study (Ando et al., 2019a). Briefly, a dried sample was placed on a metal
base with a 10-mm diameter hole in the center, then a cylindrical
plunger (3.2 mm in diameter) was inserted into the sample surface using
a universal testing machine (5542; Instron, Norwood, MA, USA) at a
speed of 1 mm s− 1 until the plunger completely penetrated the sample.
The maximum force (N), number of peaks (− ), and average drop-off (N)
were determined as indices of the mechanical properties. The number of
peaks was defined as the number of positive peaks greater than the
threshold force on the force-deformation curve. The value of the
threshold was set at 0.101 N, equivalent to 15% of the average drop-off
force value of all tested samples. The average drop-off was defined as the
average value of the drop of each positive peak (Valles-Pamies et al.,
2000). There were 10–14 replicates for each condition, and the averaged
values were used. All tests were carried out at a controlled room tem­
perature of 25 ◦ C.

2.5. Statistical analysis

Statistical analyses were performed using R software version 4.3.0 (R

Core Team). The results are presented as the means ± standard error.
Differences among mean values were compared by Tukey’s multiple
range test with analysis of variance at a significance level of p < 0.05.
Principal component analysis (PCA) was applied to characterize the
relationships between the parameters of the three-dimensional pore
structures and the mechanical properties of each dried sample.

Fig. 2. Changes in the moisture content of the apple samples during

Fig. 1. Illustration of the overall flow of image processing. A cropped region of microwave-vacuum drying. Non-frozen (a), rapid-frozen (b), and slow-frozen
interest from the raw image (a), a denoised and binarized image (b), and the (c) samples. The data shown are the mean values of eight replicates. Bars
image after pore segmentation (c). denote the standard deviation.

3
Y. Ando and D. Nei Journal of Food Engineering 369 (2024) 111944

drying times at lower pressures in the MVD of shiitake mushrooms. Since

the boiling point of water decreases as the pressure decreases, it is
believed that the evaporation rate would increase, and that drying
would progress faster in a low-pressure environment even when the
same amount of microwave energy supplied. The same trend was
observed for the rapid-frozen samples, i.e., the drying time decreased as
the pressure decreased (Fig. 2b). However, the drying time was about
67%–86% that of the non-frozen samples at the same pressure level. As
shown in our previous report (Ando et al., 2019a), this is attributable to
the fact that the cell membrane and cell wall structure are damaged by
the formation of ice crystals during pre-freezing, which increases the
moisture transfer rate inside of the sample tissue. In addition, due to
exposure to the reduced pressure environment, the internal moisture of
the pre-frozen tissues began to drip out at the beginning of the MVD
process, so the initial moisture content was lower, which may also have
contributed to the shorter drying time of the pre-frozen samples. The
slow-frozen samples had even shorter drying times, ranging from 56% to
71% of those of the non-frozen samples (Fig. 2c) at the same pressure
level. It is well known that larger ice crystals form under slow-freezing
conditions than under rapid-freezing conditions (Harnkarnsujarit
et al., 2016; Ando et al., 2019d). Therefore, the shortest drying time of
slow-frozen samples was attributed to the greater damage to the tissue
by the ice crystal formation, leading to a higher moisture transfer rate
within the tissue. According to the previous reports, the drying time of
slow-frozen samples was 62%–75% for carrots (Ando et al., 2019b) and
71%–75% for potatoes (Ando and Nei, 2023) compared with non-frozen
samples, which is almost the same level as the trend in the present study.
The three-dimensional visualization images of the pore structure in
the dried sample are shown in Fig. 3. Among the NV-MVD samples
shown in Fig. 3a, the non-frozen sample showed a large number of
relatively fine internal pores, whereas the pores in the rapid- and slow-
frozen samples tended to be larger. Among the 1-kPa-MVD samples, the
non-frozen sample was markedly smaller, and the sizes of the internal
pores were significantly reduced (Fig. 3b); in contrast, the rapid- and
slow-frozen samples showed the formation of pores that were even
larger than those of the NV samples. Fig. 4 shows histograms of the
equivalent radii of the detected internal pores of the dried samples.
Among the NV-MVD samples, the histogram of the non-frozen sample
was on the finer side, indicating that smaller pores were formed,
whereas both pre-frozen samples formed relatively large pores with a
peak at about 100 μm. Here, the histogram of the slow-frozen samples
gradually decreased to almost 260 μm, while that of the rapid-frozen
samples showed a sharper peak and converged at around 230 μm, sug­
gesting that pores that were relatively small and homogenous in size
were formed when compared to those in the slow-frozen sample.
The mean and median values of the pore equivalent radii of the
rapid- and slow-frozen samples were approximately 32%–33% and 56%
higher, respectively, than those of the non-frozen samples (Table 1).
Similar trends were obtained for the other MVD samples, although the
non-frozen 1-kPa- and 8-kPa-MVD samples showed higher peaks in the
smaller size areas. This was thought to be due to the significant localized
shrinkage that randomly occurs in non-frozen MVD samples, as has been
reported in our previous study (Ando et al., 2019a). Previous studies
have also shown that pre-freezing with MVD is effective for suppressing
sample deformation and the formation of a porous structure by reducing
the pressure difference between the inside and outside of the sample
tissue (Ando et al., 2019a). The reason why relatively smaller pores were
observed in the rapid-frozen samples than in the slow-frozen samples is
thought to be because the ice crystals that formed during rapid-frozen
were finer, and there was thus less severe tissue damage than when
compared to slow-freezing, as was mentioned earlier, and this dimin­ Fig. 3. Three-dimensional visualization of the internal structure of the
ished the effects of the reduced pressure differences. In the NV samples, microwave-vacuum dried sample with no vacuum (a), and under reduced
the effect of pre-freezing was limited, and the pore size of both the rapid- pressure at 1 kPa (b). Region of interest size: 1664 μm × 1664 μm × 2603 μm.
and slow-frozen samples was smaller than in the other MVD samples, Reconstructed images of the internal structure of dried samples (i), segmented
indicating that tissue damage due to pre-freezing tends to increase the pore structures (ii), and pore network model visualization (iii). MVD:
porosity in a reduced-pressure environment. Wu et al. (2007) reported microwave-vacuum drying.

4
Y. Ando and D. Nei Journal of Food Engineering 369 (2024) 111944

137.7
129.7

342.7
322.0
42.9
36.6
FD

258.4
249.8
91.5
88.8

20.3
13.7
SF

105.9
102.9

283.9
266.1
30.9
23.7
RF

239.3
227.3
76.7
71.2

23.9
16.9
AD

NF

137.4
134.2

341.2
328.6
Fig. 4. Porosity of the dried samples. MVD: microwave-vacuum drying; AD: air

37.9
31.8
SF
drying; FD: freeze drying. Bars denote the standard error (n = 3). Different
superscripts indicate significant differences (p < 0.05) between the means as
compared by Tukey’s multiple range test.

123.5
119.2

319.8
303.5
44.6
35.3
RF
that in the vacuum drying of eggplant, the lower the pressure, the less

MVD 1 kPa
the sample shrank and the more porous it became. They attributed this

Parameters of the pores and throats of the dried samples determined by image analysis. NF: non-frozen, RF: rapid-frozen, SF: slow-frozen samples.

205.1
195.1
to the fact that the pressure difference between the inside and outside of

36.3
24.6

18.9
16.0
NF
the sample, which induces the contraction stresses that lead to drying
shrinkage, is reduced in a vacuum environment. This means that
depressurization itself also contributes to the higher porosity, which is

153.7
152.8

370.0
349.2
51.7
47.7
the reason for the relatively low porosity of the NV-MVD samples in this

SF
study. Similar to the MVD samples, the AD samples showed a higher
peak for the non-frozen samples, but the mean and median equivalent

267.5
249.6
diameters tended to be higher than those in the MVD samples, indicating

81.4
73.5

31.8
24.1
RF
that sample shrinkage during MVD without pre-freezing was more se­

MVD 3 kPa
vere than that in AD. However, the difference in the pore size distribu­
tion between the pre-frozen samples and the non-frozen samples was

257.0
245.9
68.6
63.3

24.1
18.0
small, and the effect of pre-freezing was not as pronounced as in MVD NF
under reduced pressure. This difference was made because in MVD, the
sample becomes porous by the high vapor pressure generated from the 138.7
136.7

339.5
323.3
center of the sample by microwave irradiation, which causes the pores to

36.5
27.6
SF

expand, whereas this effect is not possible in AD. This hypothesis can be
supported by the study of Pu and Sun (2015), who confirmed by
hyperspectral imaging that moisture evaporation proceeds from the
100.4

280.2
267.4
95.8

33.3
24.6

center of the sample. The pore size distribution of the FD samples was
RF

gently distributed down to about 300 μm, and the mean and median
MVD 8 kPa

sizes were similar to those of the slow-frozen MVD samples under

222.2
213.0

reduced pressure.
25.4
19.3

13.0
10.2
NF

Fig. 5 shows the porosity of each dried sample. Among the MVD
samples, the non-frozen samples showed lower porosity, especially the
8-kPa and 1-kPa samples that exhibited significant shrinkage during
110.6
106.4

295.8
278.7
25.3
19.7

drying. Even in the pre-frozen samples, the rapid-frozen 3-kPa sample

SF

showed significantly lower porosity, which deviated from the general

trend. As discussed in the previous report (Ando et al., 2019a), the
272.9
254.7
MVD Non-vacuum

marked sample shrinkage that occurs randomly during MVD is due to

93.7
90.5

24.7
17.7
RF

the pressure difference between the inside and outside of the sample
tissue. This randomness of the shrinkage is attributed to the randomness
of the water vapor generation and microwave heating during drying.
252.9
241.0
71.1
68.1

22.3
16.5

Although to a lesser extent than non-frozen samples, rapid-freezing may

NF

have resulted in random sample shrinkage due to the relatively small

tissue damage. The pre-frozen samples generally had higher porosity
Equivalent radius

Equivalent radius

than the non-frozen samples, and the slow-frozen samples had signifi­
Channel length

cantly higher porosity values than the rapid-frozen samples. The

median (μm)

median (μm)

median (μm)
mean (μm)

mean (μm)

mean (μm)

porosity of the slow-frozen MVD samples under reduced pressure was

similar to that of the FD samples. In the slow-freezing, where tissue
damage is greater, water vapor can easily pass through and the pressure
difference within the tissue is significantly reduced, resulting in stable
suppression of sample shrinkage, which is a major advantage of
Table 1

Throat

slow-freezing pretreatment.
Pore

5
Y. Ando and D. Nei Journal of Food Engineering 369 (2024) 111944

Fig. 5. Histograms of the equivalent radius of the detected internal pores of the dried samples. MVD: microwave-vacuum drying; AD: air drying; FD: freeze drying.

Among the AD samples, although porosity was also higher in the pre-
frozen samples than in the non-frozen samples, there was no significant
difference between the rapid- and slow-frozen samples. As a general
trend, dried samples with larger pore sizes had higher porosity. The
mean and median values of the throat equivalent radius and channel
length are shown in Table 1. These two parameters play important roles
in the connectivity of pores in dried samples, and both showed a trend
similar to that of the pore equivalent radius. The channel length in­
dicates the distance between the centers of pores; therefore, the larger
the pore size, the longer the channel length. However, the NV-MVD and
AD samples showed relatively low throat equivalent radii when
compared to the pore sizes, indicating that the pore connectivity was

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Y. Ando and D. Nei Journal of Food Engineering 369 (2024) 111944

low in these samples. In general, samples with higher pore connectivity

have a larger throat equivalent radius. Therefore, this result suggests
that pore connectivity tends to be increased in MVD under reduced
pressure when compared to NV-MVD and AD. As mentioned above,
since water evaporation proceeds rapidly in MVD under reduced pres­
sure, high vapor pressure is generated inside the sample tissue, causing
pores to expand. This process may also result in a porous structure that
leads to a higher connectivity of pores.
The results of the mechanical parameters examined by the puncture
test are shown in Fig. 6. The maximum force among the MVD samples
was highest in the non-frozen NV and 8-kPa samples. Among the rapid-
frozen MVD samples, although the 3-kPa sample did not differ from the
non-frozen sample, the maximum force of the other samples was
significantly lower than that of the non-frozen samples. Furthermore,
the maximum force of the samples from slow-frozen MVD under reduced
pressure was about half of that of the rapid-frozen samples, and those
processed under lower pressure tended to have a smaller maximum
force. Previously reported data for kiwifruit at 1 kPa MVD showed that
the maximum force of slow-frozen samples was 32%–42% of that of non-
frozen samples (Ando and Okada, 2023), or about the same level as the
data at 1 kPa in this study, which was 39%, suggesting that the effect of
reducing the maximum force can be obtained for other samples. Among
all dried samples, the maximum force of the FD samples was the lowest;
however, there was no significant difference between the slow-frozen
1-kPa-MVD samples. Overall, samples with a higher porosity and
larger pore size tended to exhibit a lower maximum force. Many pre­
vious studies have suggested a relationship between the pore structure
and the maximum force (hardness) of dried foods (Xu et al., 2020;
Rizzolo et al., 2014; Thuwapanichayanan et al., 2011) that is consistent
with the result obtained in this study.
Among the MVD samples, the slow-frozen samples had a significantly
higher number of peaks than the non-frozen and rapid-frozen samples
for each pressure condition, and the number of peaks was similar to that
of the FD samples (Fig. 6b). The number of peaks for the non-frozen
samples was less than half of that for the slow-frozen samples, and the
number of peaks for the rapid-frozen samples was slightly higher than
that for the non-frozen samples, although the difference was not sig­
nificant. All AD samples showed low values, especially the non-frozen
samples, which showed significantly lower values. In contrast to the
number of peaks, the average drop-off of the MVD samples tended to be
higher among the non-frozen and rapid-frozen samples; in particular, it
was remarkably high for the rapid-frozen 8-kPa sample and the non-
frozen 1-kPa sample (Fig. 6c). The value of the slow-frozen samples
was comparable at NV and 8 kPa, but it tended to decrease as the pro­
cessing pressure decreased. In contrast, the non-frozen samples tended
to have a higher average drop-off as the pressure decreased. These
trends appeared to be inversely related to those of the porosity and pore
size. The previous study reported that a significant reduction in the
average drop-off due to pre-freezing was observed in the MVD of kiwi­
fruit at 1 kPa controlled at 30 and 40 ◦ C, whereas the effect was not
observed at 20 ◦ C (Ando and Okada, 2023). This suggests that sufficient
microwave power is required to achieve this effect, as well as the low
Fig. 6. Mechanical parameters of the dried samples as determined by the
pressure.
puncture test: maximum force (a), number of peaks (b), and average drop-off
The number of peaks and average drop-off are often associated with (c). MVD: microwave-vacuum drying; AD: air drying; FD: freeze drying. Bars
crispness (Dogan and Kokini, 2007). Valles-Pamies et al. (2000) studied denote the standard error (n = 10–14). Different superscripts indicate signifi­
the correlation between the results of sensory measurements of crispness cant differences (p < 0.05) between the means as compared by Tukey’s multiple
and instrumentally measured mechanical properties of extruded starch range test.
products, and found that a low number of peaks and high average
drop-off correspond to a crackly sample, a high number of peaks and low to have a crackly texture, and the AD samples, which had a smaller
average drop-off correspond to a crispy sample, and low values for both number of peaks and average drop-off, were considered to have a harder
parameters correspond to a hard product. In light of their study, the texture.
slow-frozen MVD samples, especially those processed at a low pressure, To analyze the relationship between the characteristics of the three-
can be categorized as crispy samples due to the high number of peaks dimensional pore structure and the mechanical parameters of the dried
and low average drop-off values as well as the FD sample. In comparison samples, PCA was performed with the determined parameters. Fig. 7a
to these samples, the non-frozen and rapid-frozen samples had a lower shows the PCA score plot of the first two principal components (PC1 and
number of peaks and higher average drop-off, and were thus considered

7
Y. Ando and D. Nei
Fig. 7. Results of PCA. PCA score plot of the first two principal components (a), and PCA loading plot of the first two principal components (b). MVD: microwave-
vacuum drying; AD: air drying; FD: freeze drying.
PC2) of the dried samples. The results of the PCA of each dried sample
showed that 73.0% and 15.0% of the total variation could be explained
by PC1 and PC2, respectively. In total, 88.0% of the variation in the data
could be explained by these two principal components, suggesting that
they were sufficient for classifying the dispersibility of the dried sam­
ples. Factor loadings of the PCA for the dried samples are shown in
Table 2. The PC1 was mainly characterized by the pore equivalent
radius, throat length, porosity, and throat equivalent radius, which
indicated that PC1 reflects structural differences in the dried samples.
The samples with high PC1 scores were the FD samples and the slow-
frozen MVD samples, which showed large pores and porous structures,
with the exception of the slow-frozen NV samples. On the other hand,
the samples with low PC1 scores were those with significant shrinkage
and low porosity, such as the non-frozen MVD samples at 8 kPa and 1
kPa. Comparisons of the MVD samples revealed that the PC1 values
tended to be divided by the pre-freezing conditions, not the pressure
conditions, and the score was high in the slow-frozen samples and low in
the non-frozen samples. The score of the rapid-frozen samples was in
between those of the slow-frozen and non-frozen samples. The PC2 was
primarily characterized by the average drop-off, and secondly charac­
terized by the maximum force and number of peaks, which indicated
that PC2 reflects the differences in the mechanical properties. The PC2
scores tended to be higher for the AD and FD samples, and lower for the
MVD samples, especially the rapid-frozen samples at 8 kPa that showed
a significantly high average drop-off. The PCA loading plot in the PC1-
PC2 plane showed that the porosity and maximum force have vectors
with opposite directions, and are thus inversely related (Fig. 7b). This
was consistent with the fact that the porosity and maximum force have
an inverse correlation, which has been suggested in previous studies as
mentioned above (Xu et al., 2020; Rizzolo et al., 2014; Thuwapa­
nichayanan et al., 2011).
Among the mechanical properties, the number of peaks and throat
equivalent radius had similar vectors, indicating a high correlation. The
throat equivalent radius indicates the size of the diameter of the contact
surface between pores, and is larger when pores are in close contact with
Table 2
Factor loadings of the principal component analysis of dried samples.
PC1 PC2
Porosity 0.40 0.03
Pore equivalent radius 0.44 − 0.07
Throat equivalent radius 0.39 − 0.25
Throat channel length 0.43 − 0.17
Maximum force − 0.37 − 0.35
Number of peaks 0.35 − 0.35
Average drop-off − 0.23 − 0.81
8
Journal of Food Engineering 369 (2024) 111944
each other and the walls separating the pores are thin, and when the
pores are larger. The throat equivalent radius was large for the FD
samples and slow-frozen MVD samples, and the fragile structure of these
samples was considered to contribute to the number of peaks. The PC1,
which depends on pore structural factors, was similar between the FD
samples and slow-frozen MVD samples, suggesting that they have a
similar pore structure. However, among these samples, the differences in
PC2, which is characterized primarily by mechanical properties, sug­
gested that there are factors other than the pore structure that influence
the mechanical properties. In the case of freeze-drying, since drying
proceeds by sublimation of ice crystals, little shrinkage occurs and there
is few difference in pore characteristics between the center and surface
layers, whereas in the case of MVD, since drying is by evaporation of
water, shrinkage of the sample surface layer is inevitable. Therefore, to
clarify the factors that characterize the texture of dried foods, an anal­
ysis that takes into account more factors should be conducted, such as
the pore structure of the surface layer since the structural evaluation in
this study was performed only for the center part of the samples, as well
as the characteristics of the walls that form pores, and the components of
the dried samples.
4. Conclusions
In the present work, apple samples were pre-frozen at different
freezing rates (slow- or rapid-freezing) and dried by MVD at different
pressure conditions (NV or at 1, 3, or 8 kPa) to investigate the quality
attributes of the dried samples. The pre-frozen samples had a shorter
drying time than the non-frozen samples at all pressure conditions, but
the rapid-freezing was less effective than the slow-freezing in reducing
the drying time. X-ray CT observations of the internal pore structure
showed that the pre-frozen MVD samples had larger pores and higher
porosity than the non-frozen samples. The pore size and porosity were
highest in the slow-frozen MVD samples, and were comparable to those
of the FD samples. The maximum force from the puncture test showed a
negative correlation with the porosity of the dried samples, and was
lower in the slow-frozen samples than in the non-frozen and rapid-
frozen samples; it also tended to be lower under the lower pressure
conditions. The slow-frozen MVD samples, especially those processed at
a low pressure, showed a high number of peaks and low average drop-off
values, indicating a crispy texture. These trends were similar to those
seen in the FD samples. The results of PCA showed that the PC1 values,
which mainly reflect the structural properties of pores, tended to be
divided by the pre-freezing conditions in the MVD samples, and not by
the pressure conditions. Although the PC1 values for the slow-frozen
MVD samples were similar to those of the FD samples, there was a
clear difference between the two in the PC2 values, which mainly reflect
Y. Ando and D. Nei
the mechanical properties, suggesting that there are factors other than
pore structure that influence the mechanical properties.
This study showed that the combination of slow-freezing pretreat­
ment with MVD under a lower pressure is advantageous for obtaining
dried products with a more porous structure. Although the mechanism
of pore formation during the drying process is still unclear, real-time
computer vision technologies developed in recent years may help to
clarify it (Aghbashlo et al., 2014). The MVD with pre-freezing technique
can be used immediately for industrial applications by using existing
practical MVD equipment. The knowledge obtained in this study on the
effects of different pre-freezing and pressure conditions on drying time,
pore structure and mechanical properties will be useful in estimating the
productivity and designing the quality of the final products. However,
more factors need to be taken into account in future analyses to clarify
the factors that characterize the texture of dried foods. For instance, it
will be necessary to evaluate the pore structure of the surface layer of
dried samples, since the structural evaluation in this study was per­
formed only for the center part of the samples. The characteristics of the
walls that form pores, and the components of the dried samples also
need to be considered as important factors. Since the instrumentally
measured mechanical properties do not necessarily directly link with the
sensory perception, it will be necessary to incorporate the study of
consumer acceptability through the sensory evaluation. Furthermore,
because of the limitations of evaluating the effectiveness of the tech­
nique based on results obtained from apples alone, a detailed study
involving other food samples should be performed in further research.
Funding
This work was supported by the Moonshot Research and Develop­
ment Program for Agriculture, Forestry and Fisheries of the Government
of Japan’s Cabinet Office (funding agency: Bio-oriented Technology
Research Advancement Institution), grant number: JPJ009237.
CRediT authorship contribution statement
Yasumasa Ando: Conceptualization, Data curation, Formal analysis,
Funding acquisition, Investigation, Writing - original draft. Daisuke
Nei: Data curation, Funding acquisition, Investigation, Writing - review
& editing.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
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