Future Foods 5 (2022) 100117

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Future Foods
journal homepage: www.elsevier.com/locate/fufo

Low-temperature vacuum drying as novel process to improve papaya

(Vasconcellea pubescens) nutritional-functional properties
Antonio Vega-Gálvez a, Elsa Uribe a,b, Alexis Pastén a,∗, Macarena Vega a, Jacqueline Poblete a,
Cristina Bilbao-Sainz c, Bor-Sen Chiou d
a
Food Engineering Department, Universidad de La Serena, Av. Raúl Bitrán, 1305 La Serena, Chile
b
Instituto de Investigación Multidisciplinar en Ciencia y Tecnología, Universidad de La Serena, Av. Raúl Bitrán, 1305 La Serena, Chile
c
Healthy Processed Foods Research, U.S. Department of Agriculture, Albany, CA, United States
d
Bioproducts Research Unit, U.S. Department of Agriculture, Western Regional Research Center, Albany, CA 94710, United States

a r t i c l e i n f o a b s t r a c t

Keywords: A novel dryer operating at low temperatures under vacuum conditions was used to study the drying kinetics and
Biological activity resulting physical and nutritional-functional properties of papaya (Vasconcellea pubescens). Drying experiments
Caricaceae were carried out at 10, 20, 30 and 40°C and constant vacuum (1 kPa). Proximate composition, dietary fiber con-
Low-temperature drying
tent, color and non-enzymatic browning changes were determined. The drying time of the fruit was significantly
Vasconcellea pubescens
influenced by the temperatures. After drying, proximate and dietary fiber compositions slightly varied in value.
Dried samples were brighter and exhibited low Maillard potential. The retention percentages of dried samples
at different drying temperature with respect to the fresh sample ranged from 71.8 to 131.3 % for total phenolic
content (TPC), 73.7 to 137 % for 𝛽- carotene content, 76.1 to 85.5 % for vitamin C content and 48.7 to 86.9 %,
for total flavonoids content (TFC). Antioxidant properties of papaya decreased significantly after drying. Overall,
this study demonstrated that low temperature vacuum drying (LTVD) improved the retention of dried papaya
bioactive compounds. However, the combination of this drying technique with other techniques is suggested to
improve drying rate.

1. Introduction
Fruits contain large amounts of nutrients and water, which make
them susceptible to deterioration by microorganisms. Drying is one com-
mon way to remove water from fruits and to prevent the microorgan-
isms from multiplying (Lenaerts et al., 2018). However, the use of high
drying temperatures causes structural, physical and mechanical modifi-
cations that might affect the chemical and nutritional quality of fruits
(Ozuna et al., 2014). Therefore, the use of low temperature drying can
provide an interesting alternative to reduce the quality changes pro-
duced by conventional drying. The most popular low temperature dry-
ing methods are low temperature convective drying and atmospheric
freeze-drying (Santacatalina et al., 2014; 2016b). In both methods, low
temperature air is used at atmospheric pressure, with water removal oc-
curring by sublimation during freeze-drying (Santacatalina et al., 2014).
However, atmospheric pressure and low temperatures retard the dehy-
dration process due to low drying rates (Ozuna et al., 2014). To over-
come this limitation, a vacuum system can be incorporated into the low
temperature drying process. This system reduces the vapor pressure of
water in the space surrounding the product as well as keep the temper-
ature of the product low (Santacatalina et al., 2014). The main use of
this technology is vacuum freeze-drying, in which the pressure must be
reduced below 6.1 kPa for sublimation to occur. The product must be
pre-frozen to the glass transition temperature of the maximally criocon-
centrated matrix, which increases the processing costs (Shofian et al.,
2011; Lenaerts et al., 2018). Thus, vacuum freeze-drying is only appro-
priate for high value and high quality products (King and Su, 1993).
Low temperature vacuum drying (LTVD) can be used to produce
products with similar characteristics to those of vacuum freeze-drying,
but at a lower cost (King et al., 2001; Caro-Corrales et al., 2005). In this
technique, the food product can be kept at low temperatures without
the need for freezing (King et al., 1989; King and Su, 1993), resulting in
a marked reduction in expenses (King et al., 1989). The first scientific
work on the LTVD technique was published by King et al. (1989) and
it was presented as a variant of controlled freezing-point food storage.
But this technique utilizes pressure just above the triple point of water
to decrease the moisture content of the material (Bauer et al., 2012). Un-
der these conditions, the LTVD technique can be operated at low tem-
peratures and the boiling point of water decreases with a decrease in
pressure (King and Zall, 1992; King and Su, 1993). In addition, the use

∗
Corresponding author.
E-mail address: afpasten@userena.cl (A. Pastén).

https://doi.org/10.1016/j.fufo.2022.100117
Received 23 August 2021; Received in revised form 5 January 2022; Accepted 17 January 2022
2666-8335/© 2022 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/)
A. Vega-Gálvez, E. Uribe, A. Pastén et al.
of vacuum also increases the drying rate by accelerating the transfer of
water (Vieira da Silva Júnior et al., 2018). This drying technique was
initially used on a model food system (King et al., 1989). The authors
demonstrated that LTVD had certain advantages compared to freeze-
drying and vacuum drying in terms of product quality and energy sav-
ings. Later, King and Chen (1998) and King et al. (2001) studied the rates
of myoglobin degradation and lipid oxidation in meat as well as chloro-
phyll degradation in spinach when using LTVD. They found lower degra-
dation of evaluated components for products using LTVD than those
using freeze-drying. Another study examined the effects of LTVD and
tunnel drying on bulk density, water adsorption and total color differ-
ence of mashed potatoes (Caro-Corrales et al., 2005). The authors found
that LTVD yielded products with lower shrinkage and clearer color than
those obtained by tunnel drying.
LTVD was developed to preserve sensitive food ingredients
(King et al., 1989), but there have been few studies of LTVD for fruits
and vegetables. One potential candidate for LTVD is Chilean papaya
(Vasconcellea pubescens). This fruit contains significant amounts of vi-
tamin C (0.495 mg g−1 ), 𝛽-carotene (162.9 𝜇g 100 g−1 ) and phenolic
compounds (0.432 mg GAE g−1 ) (Vega‑Gálvez et al., 2019). However,
the thermal instability of these compounds can result in considerable
loss during conventional drying at high temperatures. Recently, Vega-
Gálvez et al. (2021b) showed the effect of LTVD at 20 °C on antioxidant
and antimicrobial properties of V. pubescens. In the current study, the
potential of low temperature vacuum drying to preserve papaya (Vas-
concellea pubescens) was evaluated at 10, 20, 30 and 40 °C by studying
the drying kinetics and the physical and nutritional-functional proper-
ties of the final dried product.
2. Materials and methods
2.1. Raw material
Chilean papaya (Vasconcellea pubescens) was provided by a local sup-
plier in the Elqui Valley, Coquimbo, Chile. All samples had achieved
commercial maturity to minimize the variability of the raw material.
The fruits were completely washed before being peeled by immersion
in a hot solution of NaOH (10 %) and Peel 500 (1 %; Quinta industrial
Ltda., Viña del Mar, Chile) for 40 s. Peel 500 was used as an additive to
caustic solutions to accelerate the peeling process of the fruits. Skin re-
mains were removed with abundant cold water. After peeling, the seeds
and mucilage were removed and the fruit was cut into 9.0 × 1.5 × 0.4
cm slices (Vega-Gálvez et al., 2019). The slices were stored at 4 °C until
further use.
2.2. Drying experiments
Drying experiments were carried out in a cooled vacuum oven (Mem-
mert, model VOcool 400, Schwabach, Germany). The dryer was com-
posed of a compact Peltier cooling unit, combined heating and cooling
shelf and a vacuum pump. The Peltier cooling unit was only operational
when temperatures were below room temperature (<20 °C). Further de-
tails of the dryer can be found elsewhere (www.memmert.com).
The drying experiments were conducted at 10, 20, 30 and 40 °C at
constant vacuum (1 kPa). When the surface temperature of the shelf
reached the set value, 300 g samples of papaya slices were spread on
the shelf. Then the vacuum pump was started to expel the air in the
drying chamber. The experiment was continued under vacuum until the
solenoid valve was turned on.
Finally, the dried papaya slices were milled using a basic analytical
mill (IKA A-11 basic, Wilmington, USA) and sieved with a mesh of 35
(U.S. Standard Sieve Series, Dual Manufacturing Co., Chicago, ILL, USA)
to obtain 500 𝜇m particles. The powdered samples were packed in flexi-
ble high-density polyethylene bags, heat sealed and stored at 5 °C in the
dark until further use.
2
Future Foods 5 (2022) 100117
2.3. Mathematical modeling of drying kinetics
The moisture ratio (MR) of papaya slices during the drying experi-
ments was calculated using Eq. (1):
𝑀𝑡 − 𝑀𝑒
𝑀𝑅 = (1)
𝑀0 − 𝑀𝑒
where Mt is the moisture content of the papaya sample at time t, M0 is
the initial moisture content of the sample and Me is the moisture content
of the sample when its mass did not change during drying (Zhao et al.,
2021). All moisture contents were expressed as g water/g dry matter
(d.m.).
The drying rate (DR) curves of papaya slices were expressed as the
amount of mass losses per unit time (g moisture/min). It was determined
using Eq. (2):
𝑀𝑡 − 𝑀𝑡+Δ𝑡
𝐷𝑅 = (2)
Δ𝑡
where Mt is the moisture content of the sample at time t, Mt + Δt is the
moisture content of the sample at time t + Δt and Δt is the time differ-
ence (min).
Eq. (3) can be used to determine the effective diffusivity of mois-
ture assuming the diffusivity is constant, the papaya slice had a uniform
moisture distribution at the beginning of drying, the sample did not
shrink during drying and the sample can be treated as an infinite slab
(Thuwapanichayanan et al., 2011):
( ( ) )
8 𝜋 2 ⋅ 𝐷𝑒𝑓 𝑓 ⋅ 𝑡
𝑀𝑅 = 𝑒𝑥𝑝 − (3)
𝜋2 4𝐿2
where MR is moisture ratio (dimensionless), Deff is the effective mois-
ture diffusion coefficient (m2 /s), t is the drying time (s) and L is the
half-thickness of the slice (m). It should be noted that Deff is a complex
parameter that represented the different transport mechanisms, such as
molecular diffusion, liquid diffusion through the solid pores, vapor dif-
fusion, capillarity and other mechanisms that affect both DR and mass
transport (Carvalho et al., 2021), such as vacuum effects.
In addition, the drying data (MR versus time) were modeled using
seven different empirical models shown in Table 1.
2.4. Proximate composition determination
The Association of Official Analytical Chemists (AOAC, 1996) meth-
ods were used to determine moisture, fat, ash, crude protein and crude
fiber contents of the papaya samples. Water activity (aw ) was performed
using a dew point water activity analysis instrument (AquaLab 4 TE,
Pullman WA, USA) at 25 °C. All measurements were performed in trip-
licate.
2.5. Total, insoluble and soluble dietary fiber analysis
The dietary fiber content was determined according to the AOAC
991.43 (see p. 32.1.17) method using the Total Dietary Fiber Assay Kit
(TDF100A; Sigma- Aldrich, St. Louis, MO) and an enzymatic digestion
unit and filtration system (VELP Scientifica, GDE - CSF6, Usmate, Italy).
Total dietary fiber (TDF) was determined as the sum of insoluble dietary
fiber (IDF) and soluble dietary fiber (SDF). All measurements were done
in duplicate and SDF and IDF residues were corrected for protein, ash
and blank.
2.6. Color evaluation
The color of each sample was determined using a colorimeter
(HunterLab, MiniScanTM XE Plus, Reston, VA, USA). The colorimeter
was based on the CIELab method (CIE L∗ , a∗ and b∗ values, representing
whiteness/brightness, redness/greenness and yellowness/blueness, re-
spectively) at standard illuminant D65 and 10° observer angle. Six mea-
surements were carried out on a 1-cm layer of powered papaya covered
A. Vega-Gálvez, E. Uribe, A. Pastén et al. Future Foods 5 (2022) 100117

Table 1
Mathematical models applied to drying curves of Vasconcellea pubescens.

Drying temperatures (°C)

Model Parameters
10 20 30 40

Midilli-Kucuk Equation MR = a exp(-ktn ) + bt

a 0.970 ± 0.003 0.967 ± 0.006 0.969 ± 0.003 0.978 ± 0.002
k 3.83 × 10−5 ± 0.00 8.06 × 10−5 ± 0.00 1.25 × 10−4 ± 0.00 1.97 × 10−4 ± 0.00
b -1.90 × 10−5 ± 2.20 × 10−7 -1.81 × 10−5 ± 8.80 × 10−6 -2.91 × 10−5 ± 4.80 × 10−6 -2.84 × 10−5 ± 1.50 × 10−5
n 1.303 ± 0.011 1.389 ± 0.070 1.407 ± 0.066 1.390 ± 0.0612
RMSE 0.0161 0.0225 0.0358 0.0131
𝜒2 0.0003 0.0005 0.0014 0.0002
adj R2 0.9978 0.9984 0.9983 0.9987
Logarithmic Equation MR = a exp(-kt) + c
a 1.370 ± 0.009 1.240 ± 0.096 1.231 ± 0.051 1.232 ± 0.133
k 3.00 × 10−4 ± 0.00 9.67 × 10−4 ± 0.00 1.47 × 10−3 ± 0.00 1.73 × 10−3 ± 0.00
c -0.360 ± 0.010 -0.210 ± 0.097 -0.190 ± 0.048 -0.195 ± 0.1325
RMSE 0.0311 0.0251 0.0263 0.0250
𝜒2 0.0011 0.0007 0.0007 0.0007
adj R2 0.9962 0.9943 0.9935 0.9947
Verma Equation MR = a exp(-kt) + (1-a) exp(-ct)
a -7.94 × 105 ± 2.57 × 105 -1.96 × 106 ± 3.14 × 106 1.53 × 106 ± 2.90 × 106 7.92 × 105 ± 2.00 × 106
k 5.00 × 10−4 ± 0.00 1.30 × 10−3 ± 0.00 1.97 × 10−3 ± 0.00 2.27 × 10−3 ± 0.00
c 5.00 × 10−4 ± 0.00 1.30 × 10−3 ± 0.00 1.97 × 10−3 ± 0.00 2.27 × 10−3 ± 0.00
RMSE 0.0672 0.0556 0.0628 0.0573
𝜒2 0.0049 0.0033 0.0043 0.0036
adj R2 0.9645 0.9769 0.9627 0.9709
Weibull Equation MR = exp [- (t/𝜷)𝜶 ]
𝛽 1782 ± 23.26 728.7 ± 104.7 492.7 ± 32.35 412.3 ± 65.86
𝛼 1.258 ± 0.025 1.257 ± 0.041 1.348 ± 0.027 1.361 ± 0.046
RMSE 0.0586 0.0421 0.0350 0.0418
𝜒2 0.0037 0.0019 0.0013 0.0019
adj R2 0.9559 0.9759 0.9716 0.9455
Two term Equation MR = a exp(-k1 t) + b exp(-k2 t)
a 0.558 ± 9.50 × 10−4 0.569 ± 9.25 × 10−3 0.587 ± 8.91 × 10−3 0.564 ± 9.86 × 10−3
k1 5.00 × 10−4 ± 0.00 1.40 × 10−3 ± 0.00 2.17 × 10−3 ± 0.00 2.47 × 10−3 ± 0.00
b 0.510 ± 0.002 0.509 ± 0.004 0.509 ± 0.002 0.513 ± 0.003
k2 5.00 × 10−4 ± 0.00 1.40 × 10−3 ± 0.00 2.17 × 10−3 ± 0.00 2.47 × 10−3 ± 0.00
RMSE 0.0649 0.0491 0.0545 0.0496
𝜒2 0.0046 0.0025 0.0008 0.0027
adj R2 0.9703 0.9753 0.9721 0.9781
Exponential Equation MR = a exp(-kt) + (1-a) exp(-kat)
Two-Terms a 1.891± 0.003 1.596 ± 0.071 1.926 ± 0.038 1.615 ± 0.535
k 7.00 × 10−4 ± 0.00 1.73 × 10−3 ± 0.00 2.90 × 10−3 ± 0.00 2.97 × 10−3 ± 0.00
RMSE 0.0418 0.0341 0.0309 0.0310
𝜒2 0.0019 0.0012 0.0010 0.0010
adj R2 0.9880 0.9843 0.9910 0.9879
Modified Page Equation MR = exp[-(kt)n ]
k 5.61 × 10−4 ± 0.00 1.39 × 10−3 ± 0.00 2.04 × 10−3 ± 0.00 2.46 × 10−3 ± 0.00
n 1.258 ± 0.025 1.257 ± 0.041 1.348 ± 0.027 1.361 ± 0.0460
RMSE 0.0586 0.0421 0.0411 0.0418
𝜒2 0.0037 0.0019 0.0018 0.0019
adj R2 0.9559 0.9759 0.9716 0.9455

by a devise to prevent light scattering. Total color difference (∆E) was R, Tuttlingen, Germany). The supernatant was extracted, diluted 1:1
calculated by using the following expression: with 95 % ethanol, homogenized and centrifuged again. The absorbance
√ was measured at 420 nm with a UV-VIS spectro-photometer (HALO SB-
( )2 ( )2 ( )2
Δ𝐸 = 𝐿∗ − 𝐿0 + 𝑎∗ − 𝑎0 + 𝑏∗ − 𝑏0 (4) 10, Dynamica, Australia). Results were expressed as absorbance unit
(AU) per g of sample.
where, L0 , a0 , and b0 are the chromatics parameters of fresh papaya.
The polar coordinates h∗ (hue angle) and C∗ (chroma) were determined
using: 2.8. Antioxidant potential
√( )
𝐶∗ = 𝑎∗2 + 𝑏∗2 (5) The antioxidant potential of fresh and dried papaya samples was
determined by measuring total phenolic content (TPC), total flavonoid
( )
𝑏∗ content (TFC) and antioxidant capacity. The methanolic extracts were
ℎ∗ = 𝑡𝑎𝑛−1 (6)
𝑎∗ obtained according to the method in our previous work (Vega-
Gálvez et al., 2019). Briefly, papaya samples were mixed thoroughly
2.7. Non-enzymatic browning (NEB) in 80 % aqueous methanol at a solid/liquid ratio of 1:4 (w/v). The
mixture was continuously stirred for 30 min and the supernatant was
The method described by Meydav et al. (1977) was used to determine obtained after centrifugation at 4193 × g for 3 min (Hettinch® Univer-
the degree of NEB. Dried samples were soaked in 50 mL of distillated sal 320 R, Tuttlingen, Germany). The supernatant was filtered and the
water for 24 h. Subsequently, the sample was homogenized for 1 min solid residue was re-extracted one more time. The filtered extracts were
and then centrifuged at 4,193 × g for 10 min (Hettinch® Universal 320 evaporated by a multivapor (Büchi, P-6, Flawil, Switzerland) at 37°C.

3
A. Vega-Gálvez, E. Uribe, A. Pastén et al. Future Foods 5 (2022) 100117

The final residue was reconstituted in 10 mL of a methanol–formic acid

solution (99:1).

2.8.1. TPC and TFC measurements

The Folin–Ciocalteu (FC) spectrophotometric method was used to de-
termine TPC of papaya samples. The AlCl3 colorimetric assay with some
modifications suggested by Uribe et al. (2015) was used to determine
TFC of papaya samples. Measurements were performed using a VIS spec-
trophotometer (Spectronic R20 GenesysTM131, Illinois, USA) at 725nm
for TPC and 415 nm for TFC. The TPC was estimated using a calibra-
tion curve of gallic acid, whereas TFC was estimated using a calibration
curve of quercetin. Results were expressed as mg gallic acid equivalent
(GAE) or quercetin equivalent (QE) per 100 g of sample (d.m.).

2.8.2. Antioxidant capacity measurement

The anti-radical activity of papaya extracts was measured accord-
ing to the 2,2‑Diphenyl‑1‑picryl‑hydrazyl (DPPH) method developed by
Brand-Williams et al. (1995). One hundred microliters of the sample
were added to 3.9 mL of DPPH solution (50 𝜇M in methanol formic
(99:1)) and incubated in the dark for 30 min. After that, the absorbance
at 517 nm was read.
The peroxyl radical scavenging activity of papaya extracts was deter-
mined using the oxygen radical absorbance capacity (ORAC) methodol-
ogy in our previous report (Vega-Gálvez et al., 2019). A Multilabel Plate
Reader (Perkin–Elmer, VictorTM 𝜒 3 , Turku, Finland) was used for deter-
mination. In both methods, antioxidant activity was based on the stan-
dard curve of trolox and results were expressed as μmol Trolox equiva-
lent (TE) per gram of sample (d.m.).

2.9. 𝛽‑carotene and vitamin C measurements

Extraction of 𝛽‑carotene and vitamin C from fresh and dried papayas

was carried out according to our previously published method (Vega-
Gálvez et al., 2019). Measurements were performed by a HPLC system
Fig. 1. (A) The curves of moisture ratio versus drying time and (B) The curves
(Agilent 1200 series, Santa Clara, CA, USA) using the analytical condi-
of drying rate versus moisture content (d.m.) under LTVD process. Values are
tions described previously (Vega-Gálvez et al., 2019). The calibration averages (n=3) and error bars are standard deviation. 10 °C (∆), 20 °C (▴), 30
curves of 𝛽‑carotene and vitamin C were prepared in ethyl acetate and °C (◊), 40 °C (■), — Midilli–Kucuk model.
metaphosphoric acid, respectively. All analyses were carried out in trip-
licate.

2.10. 𝛼-glucosidase activity assay was calculated according to root mean square error (RMSE; Eq. (7))
and Chi-square (𝜒 2 ; Eq. (8)). The model with the lowest RMSE and 𝜒 2
The 𝛼-glucosidase activity assay described by Oboh et al. (2013) was values and the highest R2 value was identified as the model that best fit
used with minor modifications. Each well contained 50 𝜇L of papaya ex- the drying curve of the sample (Aykın-Dinçer & Erbaş, 2019).
tract in 0.1 M sodium phosphate buffer (pH 6.9) solution with 100 𝜇L ⌊ ⌋ 12
1 ∑(
N
of 𝛼-glucosidase from Saccharomyces cerevisiae (Sigma G5003, USA) (0.5 )2
RMSE = MRpre,i − MRexp,i (7)
U/mL). The plates were incubated at 20 °C for 10 min. The reaction was N i=1
initiated by adding 50 𝜇l of 4-nitrophenyl 𝛼-d-glucopyranoside (Sigma
∑N ( )2
N1377, Switzertand) in buffer. Absorbance at 405 nm was recorded ev- 2 i=1 MRpre,i − MRexp,i
χ = (8)
ery 30 s for 10 min using a Victor3 Multilabel Plate Reader set to 20 N−z
°C (Perkin–Elmer, Turku, Finland). The inhibitory property of papaya
extract against 𝛼-glucosidase was expressed as the concentration that 3. Results and discussion
inhibited 50 % of the enzyme activity (IC50).
3.1. Drying kinetics of papaya samples
2.11. Statistical analysis
The effects of LTVD on drying papaya are shown in Figure 1, with
The physical and nutritional-functional properties data were ana- plots of moisture ratio versus drying time and drying rate versus mois-
lyzed using Statgraphics Centurion XVI (Statistical Graphics Corp., Her- ture content. From Fig. 1A, a lower drying temperature led to rather long
don, VA), whereby one-way analysis of variance (ANOVA) was carried drying times (at 1 kPa vacuum pressure). The drying times required to
out and the least significant difference (LSD) intervals were identified. reduce the moisture ratio to 0.0076 at 10 °C, 0.0068 at 20 °C, 0.0002
The significance difference was measured at a confidence level of 95 % at 30 °C and 0.0001 at 40 °C were 77.6, 36.0, 22.0 and 19.5 h, respec-
(p < 0.05). tively. Papaya undergoing LTVD required a large amount of time and
Nonlinear least squares analyses of the empirical models were done energy. The experimental-scale dryer used in the current study cannot
using SigmaPlot 11.0 (Systat Software Inc. USA) to determine constants be operated at a lower vacuum pressure than 1 kPa. A vacuum pressure
for all models and the regression coefficients (R2 ). The goodness of fit as low as that used in a freeze-dryer (<0.01 kPa) may be necessary to

4
A. Vega-Gálvez, E. Uribe, A. Pastén et al.
improve the drying efficiency. Also, further research is required to com-
bine LTVD with other techniques, such as ultrasound (Krishnan et al.,
2020; Li et al., 2020), infrared (Salehi and Kashaninejad, 2018), pulsed
electric field (Liu et al., 2020) or microwave (Ali et al., 2020) to improve
the drying rate of food materials.
Fig.1B depicts the variations in drying rate and sample moisture of
papaya dehydrated by LTVD at different temperatures. The drying rate
curve of the papaya sample at 10°C consisted of an initial decreasing
rate period, a subsequent constant-rate period and a final falling drying
rate period. Interestingly, the constant drying rate period disappeared
with an increase in drying temperature. This finding was in good agree-
ment with a study on vacuum drying of hawthorn fruit juices (Li et al.,
2020). This behavior was due to the moisture diffusion rate inside the
sample being smaller than the evaporation rate on the surface, with no
constant drying rate being reached (Ali et al., 2020; Xu et al., 2020).
During the initial drying period, the samples showed a rapid decrease
in moisture values due to the vacuum drying process. Free water in sam-
ples was vaporized at low temperatures due to large vapor pressure dif-
ferences (Xu et al., 2021). As the drying process progressed, the evapo-
ration rate of free water gradually became lower and the moisture dif-
fusion process in the interior of the sample became the dominant phys-
ical mechanism (Zhao et al., 2021). However, the mechanism of mois-
ture loss was rather complex and other forces could be involved during
vacuum drying. For instance, the decrease of vacuum pressure could
generate bubbles inside samples due to the difference between the ther-
mal conductive plate temperature and the vapor saturation temperature
during the initial drying period, creating microscopic channels by split-
ting, rupturing and cracking tissues, thereby allowing moisture transfer
(Xu et al., 2021). Consequently, surface diffusion, capillary flow actions,
pressure driven flows and other mechanisms could also occur so that the
internal moisture could be more easily transferred outward (Liu et al.,
2020).
3.2. Modeling drying kinetics
Drying kinetics data for papaya slice at 10, 20, 30 and 40 °C were
fitted to seven drying models. The model constants and model selection
criteria (RMSE, 𝜒 2 and adjusted R2 ) are presented in Table 1. Although
all models successfully described the relationship between time and MR,
the Midilli-Kucuk model exhibited the best fit to the drying data. This
model had the highest R2 value and the lowest 𝜒 2 and RMSE values,
which indicated that predicted data using this model will be closer to the
experimental drying data. The Midilli-Kucuk model had been success-
fully used to model drying of papaya puree in a refractance windowTM
dryer (Ocoró-Zamora and Ayala-Aponte, 2013). The K parameter in the
Midilli-Kucuk model showed an increase in value with an increase in
temperature (Table 1). This increase could be due to the decrease in
the external resistance to water transfer at higher temperatures. Tem-
perature rise also contributed to increased evaporation rates and water
diffusion inside the sample (Santacatalina et al., 2016a). The effective
moisture diffusivity (Deff ) values of papaya slices by LTVD were found to
be 2.819 × 10−11 , 6.134 × 10−11 , 9.847 × 10−11 and 13.08 × 10−11 m2 /s
at 10, 20, 30 and 40°C, respectively. A previous study reported that Deff
values varied between 6.25–24.32 × 10−10 m2 /s for papaya slices dried
in a convective dryer at 40–80°C (Lemus-Mondaca et al., 2009). These
results confirmed that Deff of papaya samples increased in value with
an increase in temperature. Santacatalina et al. (2015) also reported
that Deff values in apples dried using a convective dryer increased 14-
fold from 4.50 × 10−11 m2 /s at –1°C to 65.81 × 10−11 m2 /s at 60°C.
Caro-Corrales et al. (2005) obtained a Deff value of 1.9 × 10−11 m2 /s for
mashed potatoes dried by LTVD (0.67 kPa). These differences in Deff val-
ues might be due to variations in the structure, composition, geometry
and moisture content of each food as well as different vacuum pres-
sures and drying temperatures used in the experiments (Aykn-Dinçer &
Erba, 2019; Zhao et al., 2021).
5
Future Foods 5 (2022) 100117
3.3. Effects of LTVD method on proximate composition and dietary fiber
contents
The proximate composition of fresh and dried papaya slices is pre-
sented in Table 2. The initial moisture content of the fresh papaya
slice was 93.49 g/100 g. The final moisture contents after drying var-
ied from 12.69 to 16.03 g/100 g on a wet basis (w.b.) after dehydra-
tion. More importantly, all drying conditions significantly reduced wa-
ter activity below 0.60 (Table 2), where microbiological growth was
inhibited. Therefore, the LTVD method was effective in reducing wa-
ter activity of samples to a safe value. The fat, ash, protein and fiber
contents of fresh papaya were within the range reported for Vascon-
cellea pubescens (on w.b. or d.m.) in earlier studies (Uribe et al., 2015;
Vega-Gálvez et al., 2019). Low temperature drying resulted in signifi-
cant differences between the fresh and processed samples (Table 2). As
the drying process progressed and moisture content decreased, the pa-
paya cellular structure became gradually destroyed with an increase in
porosity. This may lead to the variations in proximate composition of
food material after dehydration. This result was consistent with those of
Gutiérrez et al. (2008), Tenyang et al. (2017) and Lenaerts et al. (2018),
who found that structural changes in the cellular tissue of the material,
water loss and browning reactions after dehydration may lead to vari-
ations in proximate compositions. For example, the sample dried at 10
°C had the lowest fat content, which was likely due to deterioration and
oxidation of fat molecules at long drying times. Nonetheless, reduction
in fat content after LTVD was important to reduce the rancidity reac-
tions and increase the storage life of the product (Darfour et al., 2021).
A significant increase in protein content of the dried sample at 10 °C
may be attributed to the destruction of protein inhibitors (Kumar et al.,
2021). Meanwhile, the reduction in protein content (p<0.05) with an
increase in drying temperature (30 and 40 °C) might be due to ther-
mal denaturation of heat liable nitrogenous compounds such as amino
acids (Patel et al., 2019). The fresh and processed papaya at 20, 30 and
40 °C exhibited no significant (p>0.05) differences in crude fiber con-
tents. In comparison, the 10 °C sample had a significantly lower crude
fiber content, which may be attributed to the polysaccharides and their
derivatives degrading after long sample drying times.
The dietary fiber (DF) changes of papaya samples are also presented
in Table 2. Insoluble, soluble and total DF of the fresh sample was 29.91,
7.01 and 36.92 g/100 g d.m., respectively. These results were consistent
with previous studies that found more insoluble DF than soluble DF in
Vasconcellea pubescens (Vega-Gálvez et al., 2019) and dietary fiber con-
centrates obtained from Carica papaya pulp and peel (Calvache et al.,
2016).
The LTVD process had some effect on the DF fraction contents
(Table 2). For example, dried papaya at 10 °C had lower SDF content,
but higher IDF content compared to fresh papaya, whereas dried pa-
paya at 30 °C had lower IDF content. Nonetheless, the contents of TDF
in all dried samples were statistically similar (p>0.05) with the fresh
sample, indicating the LTVD process did little damage to dietary fibers
in papaya.
3.4. Effects of LTVD method on color attributes and non-enzymatic
browning
The color properties of fresh and dried papaya are shown in Table 3.
The fresh sample was characterized by high luminosity, with a tendency
toward bright yellow (L∗ = 63.7; h∗ = 82.6°; C∗ = 43.4). In comparison,
the LTVD samples had higher L∗ values, indicating they were lighter in
color than the untreated papaya samples (P < 0.05). Previous studies
(Lyu et al., 2016; Yi et al., 2017; Udomkun et al., 2018) also reported
that the L∗ values of vacuum lyophilized papaya were higher than those
of the untreated samples.
The fresh papaya had a lower a∗ value and a higher b∗ value than
those of Carica papaya reported in literature (Lyu et al., 2016; Yi et al.,
2017; Udomkun et al., 2017). This was consistent with Vasconcellea
A. Vega-Gálvez, E. Uribe, A. Pastén et al. Future Foods 5 (2022) 100117

Table 2
Effects of low temperature vacuum drying on proximate composition and dietary fiber content in Vasconcellea pubescens.

Drying temperatures (°C)

Parameters
Fresh 10 20 30 40
1
Moisture 93.5 ± 0.41a 16.0 ± 0.10b 14.7 ± 0.14c 13.5 ± 0.26d 12.7 ± 0.25e
2
Fat 2.89 ± 0.23a 1.58 ± 0.05d 2.41 ± 0.19b 2.03 ± 0.16c 2.58 ± 0.23ab
2
Ash 11.8 ± 0.39b 12.8 ± 0.07a 10.8 ± 0.21c 10.3 ± 0.48c 12.1 ± 0.49b
2
Crude protein 9.64 ± 0.30b 12.2 ± 0.88a 10.0 ± 0.21b 8.20 ± 0.51c 8.47 ± 0.14c
2
Crude fiber 15.0 ± 0.76a 13.0 ± 0.87b 14.4 ± 0.88a 14.6 ± 0.37a 14.6 ± 0.29a
3
Water activity 0.992 ± 0.003a 0.599 ± 0.015b 0.538 ± 0.006c 0.504 ± 0.005d 0.483 ± 0.004e
2
Insoluble dietary fiber 29.9 ± 0.80ab 38.6 ± 4.03a 33.7 ± 5.29ab 24.9 ± 0.57b 29.1 ± 4.76ab
2
Soluble dietary fiber 7.01 ± 0.11ab 1.67 ± 0.93d 8.57 ± 0.88a 5.49 ± 1.13bc 4.29 ± 0.46c
2
Total dietary fiber 36.9 ± 0.91ab 40.3 ± 4.97a 42.2 ± 4.40a 30.4 ± 1.69b 33.4 ± 4.30ab

Values are expressed as means ± standard deviation of triplicates. Values with different letters in the same row are significantly different (p < 0.05). 1 Expressed as
g/100 g
2
expressed as g/100 g dry matter
3
Dimensionless.

Table 3
Effects of low temperature vacuum drying on chromatic parameters and non-enzymatic browning (NEB) in Vasconcellea pubescens.

Drying temperatures (°C)

Parameters
Fresh 10 20 30 40

L∗ 63.7 ± 0.45e 80.7 ± 0.20d 81.7 ± 0.27c 82.7 ± 0.32a 82.2 ± 0.12b
a∗ 5.58 ± 0.21c 6.79 ± 0.10a 5.70 ± 0.21b 4.84 ± 0.13d 4.60 ± 0.04e
b∗ 43.1 ± 0.27a 39.8 ± 0.43b 36.6 ± 0.39c 36.4 ± 0.48c 35.5 ± 0.14d
ΔE - 17.2 ± 0.54c 19.1 ± 0.48b 20.2 ± 0.50a 20.1 ± 0.30a
h° 82.6 ± 0.27a 80.3 ± 0.09d 81.1 ± 0.23c 82.4 ± 0.14b 82.6 ± 0.05ab
C∗ 43.4 ± 0.27a 40.4 ± 0.44b 37.0 ± 0.42c 36.7 ± 0.49d 35.8 ± 0.14e
NEB (abs/g) 0.001 ± 0.000d 0.020 ± 0.002c 0.036 ± 0.002a 0.032 ± 0.001b 0.021 ± 0.001c

Values are expressed as means ± standard deviation of six replicates. Values with different letters in the same row are significantly different (p < 0.05).

Table 4
Effects of low temperature vacuum drying on bioactive compounds and antioxidant capacity of Vasconcellea pubescens.

Drying temperatures (°C)

Parameters
Fresh 10 20 30 40

Bioactive compounds
TPC, mg GAE/100 g d.m. 827 ± 67.6b 594 ± 52.2d 698 ± 50.4c 789 ± 63.0b 1086 ± 144a
TFC, mg QE/100 g d.m. 145 ± 20.3a 70.6 ± 6.69d 89.4 ± 9.44c 85.6 ± 8.19c 126 ± 12.4b
𝜷-carotene, 𝝁g/100 g d.m. 2.62 ± 0.04c 3.58 ± 0.09a 2.99 ± 0.02b 2.18 ± 0.04d 1.93 ± 0.04e
Vitamin C, mg/100 g d.m. 805 ± 28.1a 613 ± 12.7d 626 ± 26.6cd 654 ± 4.47bc 688 ± 14.5b
Antioxidant capacity
DPPH, μmol/TE g d.m. 45.8 ± 4.43a 12.2 ± 1.40e 22.4 ± 1.73d 36.0 ± 2.87b 31.6 ± 3.32c
ORAC, μmol/TE g d.m. 260 ± 12.7a 80.6 ± 6.97d 139 ± 5.26b 110 ± 3.03c 109 ± 3.87c

Values are expressed as means ± standard deviation of three replicates. Values with different letters in the same row are significantly different (p < 0.05).
Total phenolic content (TPC); Total flavonoid content (TFC); 2,2-diphenyl-1-picrylhydrazyl (DPPH); Radical Absorbance Capacity (ORAC).
Gallic acid equivalents (GAE); Quercetin equivalents (QE); Trolox equivalents (TE).

pubescens having a more yellow and much less red color compared with
Carica papaya. The 10 and 20°C samples had higher a∗ values, whereas
the 30 and 40°C samples had lower a∗ values compared to the fresh sam-
ple. The b∗ values decreased for all dried samples (Table 3). Vieira da
Silva Júnior et al. (2018) attributed this to isomerization or greater re-
tention of some types of carotenoids over others after drying. This expla-
nation was consistent with the increase in 𝛽-carotene contents in the10
and 20°C samples and a decrease in 𝛽-carotene contents in the 30 and
40°C samples (Table 4).
The dried samples had total color difference (ΔE) values that ranged
from 17.20 to 20.19, indicating color differences between the dried and
fresh samples. The samples dried at 10 °C had the lowest ΔE value, sug-
gesting that this sample was the most similar in color to fresh papaya
(Yi et al., 2017). The 40°C sample had the highest h∗ (82.62°) value, in-
dicating negligible differences compared to the fresh sample, with both
samples possessing a yellow color. However, the 40°C sample had lower
saturation index (C∗ ) value (35.84) than that of the fresh sample (43.41),
indicating the yellow of the fresh sample was vivid, whereas the yellow
of the 40°C sample was dull. Also, all dried samples had significantly
lower C∗ values than that of the fresh sample. This was probably due to
the formation of dark compounds from the degradation of phenolic com-
pounds and vitamin C during drying (Table 4) (Vieira da Silva Júnior
et al., 2018).
The dried samples had significantly (p<0.05) larger non-enzymatic
browning (NEB) values than that of the fresh sample (Table 3). This in-
crease represented the production of browning products during LTVD
and can be explained by the slight ascorbic acid degradation (Table 4).
However, the NEB values were too small to affect the lightness (L∗ val-
ues) of the dried samples (Table 3). The limited oxygen and low temper-
atures during drying probably induced release of aglycone compounds
and glucose, which reduced the Maillard potential of the generated
browning products (Alongi et al., 2018).

6
A. Vega-Gálvez, E. Uribe, A. Pastén et al.
3.5. Effects of LTVD method on bioactive compounds and antioxidant
capacity
The structure of the vacuum-dried samples can be rather hetero-
geneous, with the sample having a dried surface and a central region
saturated with water, depending on the drying temperature (Liu et al.,
2020). This can affect the amount of bioactive compounds, vitamins or
pigments. However, other factors such as drying temperature and expo-
sure time can also affect these components.
Table 4 shows the effects of LTVD on bioactive compounds and an-
tioxidant capacity of papaya slices. The fresh sample had TPC, TFC and
vitamin C values of 827 mg GAE/100 g d.m., 145 mg QE/100 g d.m.
and 805 mg/100 g d.m., respectively. These values were comparable to
those found for Vasconcellea pubescens in literature (Uribe et al., 2015;
Vega-Gálvez et al., 2019). The 10, 20 and 30°C samples had significantly
lower TPC values than that of the fresh sample, whereas the 40°C sample
had a significantly higher TPC value. Also, all dried samples had lower
TFC and vitamin C values than that of the fresh sample (Table 4). This
could be explained by the long dehydration times and the reduced in-
activation of oxidative enzymes (polyphenol oxidase, peroxidase, ascor-
bate oxidase) responsible for phenolic compound (Santacatalina et al.,
2015) and ascorbic acid degradation (Sehrawat et al. 2018) at 10, 20
and 30°C. In comparison, the 40°C sample experienced a much shorter
drying time and increased inactivation of these oxidative enzymes, lead-
ing to a higher TPC value and better retention of TFC and vitamin C.
The 𝛽-carotene content in the fresh sample was lower than those
previously reported for C. papaya (Wall, 2006; Shofian et al., 2011). A
possible reason could be that the skin and pulp of V. pubescens turned
more yellow than red upon ripening. Our results indicated that drying
at 10 and 20°C better preserved 𝛽-carotene content since this pigment
is temperature-sensitive (Table 4). The decrease in 𝛽-carotene content
with an increase in drying temperature indicated that 𝛽-carotene was
susceptible to degradation, isomerization and oxidation, especially at
high temperatures (Zhao et al., 2021). In addition, papaya slices were
not dried homogeneously by LTVD and the final moisture content of the
sample was nonuniform at the different drying temperatures. This may
also affect 𝛽-carotene content of the samples.
Several studies had examined the degradation of bioactive compo-
nents during freeze-drying of papaya (Shofian et al., 2011; Lyu et al.,
2016; Yi et al., 2017; Vega-Gálvez et al., 2019), but no pre-
vious studies had examined the effects of LTVD on polyphenol,
flavonoid, vitamin C and 𝛽-carotene contents of fruits. However,
Santacatalina et al. (2014) reported that drying apples at low tempera-
tures (-10, -5, 0 and 10 °C) led to TPC and TFC degradation, with even
greater degradation at temperatures below the freezing point.
Fresh papaya had a DPPH activity of 45.8 μmol/TE g d.m. (2.98
μmol/TE g w.b.) and an ORAC activity of 260 μmol TE/g d.m. (16.95
μmol TE/g w.b.), which were comparable to those reported in literature
(Udomkun et al., 2015; Udomkun et al., 2016; Uribe et al., 2015; Vega-
Gálvez et al., 2019). Dried samples had significantly lower antioxidant
values after LTVD treatment (p<0.05), as shown in Table 4. The DPPH
and ORAC values for the 10 °C sample decreased by 73 and 69 %, respec-
tively. This could be due to lower retention of TPC, TFC and vitamin C
at this temperature since several studies had found a strong correlation
between total phenols and antioxidant capacity (Udomkun et al., 2016).
The 40 °C sample had a higher TPC value than that of the fresh sample
and consequently, should have higher antioxidant activity. However,
this was not the case so further work is required to identify individual
bioactive compounds to explain this discrepancy.
3.6. Effects of LTVD method on 𝛼-glucosidase activity
The 𝛼-glucosidase plays a key role during the digestion of carbo-
hydrates and its inhibition is necessary for better plasma glucose man-
agement (Alongi et al., 2018). As shown in Fig. 2, extracts obtained
from dried papaya at different temperatures effectively inhibited 𝛼-
7
Future Foods 5 (2022) 100117
Fig. 2. IC 50 (half-maximal inhibitory concentration) values of papaya extracts
obtained from fresh and subjected to low temperature vacuum drying at differ-
ent temperatures. Bars with the same letter are not significantly different (p <
0.05). Values are averages (n=3) and error bars are standard deviation.
glucosidase activity. In comparison, the extract obtained from fresh pa-
paya had a high IC50 value of 401.14 mg/mL and was only weakly ef-
fective against the 𝛼-glucosidase enzyme. These results were consistent
with our previous studies, which found that extracts from dehydrated
V. pubescens by freeze-, vacuum-, solar-, convective- and infrared-drying
(Vega-Gálvez et al., 2019) and from different vacuum drying tempera-
tures (40, 50, 60, 70, and 80 °C) at a constant vacuum of 15 kPa (Vega-
Gálvez et al., 2021a) were more effective as inhibitors of 𝛼-glucosidase
than the fresh sample. The important ultrastructure changes of papaya
tissue and the alteration of the surface microstructure during vacuum
drying could promote the extraction of bioactive components from the
matrix (Liu et al., 2021). In our study, extracts from dried papaya at
10 and 20 °C were the most effective inhibitors of 𝛼-glucosidase, with
IC50 values of 16.83 and 14.92 mg/mL, respectively. The high inhi-
bition activity of these extracts might be due to their high 𝛽-carotene
contents and their synergistic effects with some papaya phenolic com-
pounds. A recent comprehensive review had highlighted the in vitro 𝛼-
glucosidase inhibition by flavonoids from fruit and vegetable extracts
(Papoutsis et al., 2021). The authors noted that hydroxylated forms of
flavanone glycosides, such as naringin, have higher inhibition activities
than their natural forms. In our previous study, we found that three
flavonoids, epicatechin, naringin and quercetin, were generated after
drying papaya (Vega-Gálvez et al., 2021b), which could explain the ef-
ficacy of drying for inhibiting 𝛼-glucosidase in vitro.
4. Conclusion
LTVD can be effectively used to protect thermally sensitive com-
pounds, such as 𝛽-carotene, since drying occurred at low temperatures.
Also, papaya dried at higher temperatures using LTVD had better reten-
tion of TPC and TFC. Moreover, dried papaya inhibited 𝛼-glucosidase ac-
tivity better than fresh papaya. However, LTVD required a large amount
of time and energy, so further research is required to effectively use this
technique in the food industry. For instance, LTVD can be used to dehy-
drate higher value foods that are heat-sensitive and have high moisture
contents. Also, LTVD can be combined with other drying techniques to
improve drying efficiency and retain the quality parameters of the sam-
ples. In addition, LTVD can be compared to freeze-drying in terms of
energy consumption and retention of fruit compounds. Eqn. (4-6)
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.
A. Vega-Gálvez, E. Uribe, A. Pastén et al. Future Foods 5 (2022) 100117

Acknowledgments Papoutsis, K., Zhang, J., Bowyer, M.C., Brunton, N., Gibney, E.R., Lyng, J., 2021. Fruit,
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𝛼-glucosidase inhibition properties: A review. Food Chem. 338, 128119.
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