LWT - Food Science and Technology 157 (2022) 113092

Contents lists available at ScienceDirect

LWT
journal homepage: www.elsevier.com/locate/lwt

Optimization of the osmotic dehydration process of plums (Prunus Salicina

Lindl.) in solutions enriched with inulin, using response
surface methodology
Irene Palacios Romero , María José Rodríguez Gómez , Francisco Manuel Sánchez Iñiguez ,
Patricia Calvo Magro *
Área de Vegetales, Instituto Tecnológico Agroalimentario de Extremadura, Centro de Investigaciones Científicas y Tecnológicas de Extremadura (CICYTEX), Avda. Adolfo
Suárez, s/n, 06007, Badajoz, Spain

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

Keywords: The objective of this work was to study the effect of an osmotic solution (containing water, glycerol and inulin)
Box-Behnken design on water loss (WL), weight reduction (WR), inulin gain (INU), glycerol gain (GLY), water activity, colour pa­
Response surface methodology rameters and mechanical properties of dehydrated plum. Only the second-degree polynomial model obtained
Inulin
using response surface methodology for WL, WR, INU and GLY proved appropriate for predicting experimental
Mass transfer
data. The optimum proportions were 522 g water, 219 g glycerol and 100 g inulin, which produced WL, WR, INU
Plums
and GLY values of approximately 30% and 29%, and 119 mg/g and 373 mg/g, respectively.

& Oszmiański, 2014). In such cases, partial moisture removal processes,

1. Introduction
In recent decades, important socioeconomic changes have taken
place, which have led to substantial changes in dietary patterns and food
consumption. In association with this, there has been a growing demand
for food that can provide nutrients and additional health benefits.
Fruit and vegetables are important components of the daily diet due
to their content of vitamins, minerals, phytonutrients, and fibre, etc.
(Porat, Lichter, Terry, Harker, & Buzby, 2018), but they are generally
highly perishable. Japanese plum (Prunus salicina L.), which is one of the
most economically important stone fruits worldwide, is highly appre­
ciated by consumers on account of its brightly coloured appearance,
characteristic taste and high nutritional value (Roussos, Efstathios,
Intidhar, Denaxa, & Tsafouros, 2015; Sahamishirazi, Moehring, Clau­
pein, & Graeff-Hoenninger, 2017). However, it is only available for a
few months each year due to its seasonality.
Conventional dehydration is probably the oldest method used to
extend the shelf life of fruit, and of plums in particular. Conventional hot
air drying (CD) is the most common approach used to remove moisture
from plant material, mainly due to its low cost (Lewicki, 2006). How­
ever, this method requires high temperatures and time, resulting in a
significant degradation of important nutrient compounds and alter­
ations in the colour of the final product (Wojdyło, Figiel, Lech, Nowicka,
like osmotic dehydration (OD), applied as pre-treatments, prior to dry­
ing, can substantially reduce negative effects and allow the creation of
new food products and the introduction of innovative technologies.
In OD, fruits (whether sliced or whole) are dehydrated by immersion
in hypertonic solutions. The main mechanisms generated during the
dehydration process involve the removal of water and certain soluble
solids from the fruit (including sugar, phenolic compounds and min­
erals) to the hypertonic solution. This is accompanied by the migration
of solutes from this solution to the inner part of the fruit (Landim,
Barbosa, & Júnior, 2016).
The osmotic solution influences the nutritional value of the foods.
The osmotic agent must be effective, convenient, non-toxic, have a good
taste, and be readily dissolvable to form a highly concentrated solution
(Yadav & Singh, 2014). Fructose, sucrose and sodium chloride are
typically used in osmotic solutions for fruit and vegetable dehydration
(Lemus-Mondaca, Noma, Igura, Shimoda, & Pérez-Won, 2014; Sri­
tongtae, Mahawanich, & Duangmal, 2011).
OD has recently been used to obtain functional foods (Nagai, Santos,
Faria, Boscolo, & Mauro, 2015; Salazar-López, Jiménez, Salazar, &
Azuara, 2015). In such cases, inulin - characterized by prebiotic prop­
erties- (Abed, Ali, Noman, & Bakry, 2016) may be used as a component
of the osmotic solution to obtain high-value food products.
In general, high solid gain during the OD process is not desirable,

* Corresponding author.
E-mail address: patricia.calvo@juntaex.es (P. Calvo Magro).

https://doi.org/10.1016/j.lwt.2022.113092
Received 9 August 2021; Received in revised form 17 December 2021; Accepted 8 January 2022
Available online 12 January 2022
0023-6438/© 2022 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
I. Palacios Romero et al. LWT 157 (2022) 113092

2.3. Osmotic dehydration process

Abbreviations
Fresh plums were cleaned and cut into slices with an approximate
WL, water loss thickness of 2.5 cm. The slices were then dipped in a 0.1% ascorbic acid
WR weight reduction solution (Panreac) for 5 min to prevent non-enzymatic browning re­
INU inulin gain actions and were then drained before the osmotic process. This process
GLY glycerol gain was carried out in a controlled shaking incubator (Model G76, New
CD Conventional hot air drying Brunswick Scientific Co. Inc., Edison, N.J. U.S.A). For OD, the plum
OD osmotic dehydration slices and the desired osmotic solution were placed in 1 L beakers and
ED-RSM experimental design and response surface methodology kept at 60 ◦ C for a standard immersion time of 240 min. Constant
W water shaking was applied to obtain a homogeneous osmotic solution and to
SG solid gain ensure a uniform distribution of temperature. To prevent evaporation
RSM surface methodology from the osmotic solution, the beakers were covered with plastic
Gly glycerol content wrapping during the experiments. The sample to solution ratio was
Inu inulin content stablish based on preliminary experiments and was maintained at 1:2
(w/w). After each experiment, the samples were rinsed with water and
then blotted with absorbent paper in order to remove the excess of os­
motic solution.
unless the objective is to enrich the product with bioactive compounds.
Although inulin has been the subject of many studies over the years,
there is only limited information available relating to the kinetic pro­ 2.4. Conventional drying
cess, in terms of water loss and solid gain, and also fruit quality
(Jiménez-Hernández et al., 2017). The aim of this work was to optimize Osmotically dehydrated plum slices obtained under these experi­
the composition of the osmotic solution by means of experimental mental conditions were then conventionally dried in a force convection
design and the application of response surface methodology (ED-RSM) oven, at atmospheric pressure, and at a temperature of 60 ◦ C, for 8 h.
to obtain dried plums enriched with inulin. For this purpose, mass
transfer (water loss, weight reduction, solids gain, inulin uptake, and 2.5. Moisture and water activity determination
glycerol uptake) and fruit quality parameters (water activity, colour,
and mechanical properties) were taken into account. The moisture content was measured gravimetrically by drying
approximately 1.0 g of samples at 105 ◦ C for 24 h. Water activity (aw )
2. Materials and methods was measured at 25 ± 1 ◦ C, using a water activity meter (Novasina
Labmaster-aw) that had been previously calibrated with a certified
2.1. Vegetal material standard solution (Novasina AG). All the experiments were carried out
in triplicate.
Fresh plums (Prunus Salicina Lindl.) variety ‘Sun Gold’, at commer­
cial maturity level and uniform size were obtained from a local pro­
2.6. Mass transfer calculations
ducer, located in “Vegas Bajas del Guadiana” (Extremadura, Spain).
Samples were stored at +1 ◦ C and at a relative humidity of 90% prior to
The water loss (WL), weight reduction (WR) and solid gain (SG)
OD treatment. For the other analysis, fresh and dehydrated samples
variables were calculated using the following equations: (1) to (3):
were stored at − 80 ◦ C. The initials moisture and soluble solid (◦ Brix)
contents of the fresh plums were 91.3 ± 0.1% and 14.74 ± 0.70 (wet WL (%) =
mi zi − mf zf
x 100 (1)
basis) respectively. mi

mi − mf
2.2. Osmotic solutions WR (%) = x 100 (2)
mi

Osmotic solutions were prepared by dissolving the required amounts mf sf − mi si

SG (%) = x 100 (3)
of glycerol (Dimensa S.L., Gly) and inulin (Fritafit TEX ®, Inu) in mi
deionized water (W) according to the Box-Behnken experimental design
(Table 1). Inulin is officially recognized as a natural food ingredient and where mi and mf are the initial and final weights (g) of the samples; zi
is classified as dietary fiber in most European countries (Roberfroid, and zf are the initial and final mass fractions of the water (g water/g
2000; Regulation (EC) N. 1924/2006/EU). Glycerol is a low molecular sample); and si and sf are the initial and final mass fractions of total
weight sugar alcohol with low sweetness which is recognized as a solids (g total solids/g sample).
non-toxic and safe additive and can be used following the principle of
quantum satis (Commission Regulation (EU) No 1130/2011). Finally, 2.7. Colour measurements
0.1% of citric acid (Panreac) was added to the osmotic medium as a
stabilizing agent. Colour measurements of fresh and conventionally dried samples
were performed using a colorimeter (Minolta, Model CR 400, Konica
Minolta Sensing, Japan) with illuminant C and an 8 mm diameter
viewing area. The colour parameters were reported in relation to the
CIELAB scale (L*, a* and b*), where L* is related to luminosity, a* refers
Table 1
to redness (+a*) or greenness (− a*), and b* indicates yellowness (+b*)
Real and coded values of independent variables for experimental design.
or blueness (− b*). Analyses were performed at room temperature and
Independent variables Coded Levels − 1 0 +1
measurements were taken directly from the skin and flesh surfaces of the
Water (g) W 500 550 600 plum slices. Sampling was performed in quintuplicate and data were
Glycerol (g) Gly 200 300 400 reported as average values. Total colour change (ΔE*) was calculated
Inulin (g) Inu 50 75 100
according to Eq. (4):

2
I. Palacios Romero et al.
√̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
( )2 ( )2
L* − L*0 + (a* − a*0 ) + b* − b*0
2
ΔE =
where L∗0 , a∗0 and b∗0 respectively represent the readings taken from a
fresh sample.
2.8. Mechanical property evaluation
The textures of fresh and conventionally dried samples were ana­
lysed by uniaxial compression, using a Texture Analyzer (TA.XT2i),
(Surrey, England). Values for stress and strain at failure were deter­
mined using a lubricated acrylic plate with a 25 mm diameter, at a
crosshead speed of 1 mm s− 1, until 80% sample deformation. Ten-mm-
diameter cylindrical samples were collected from the centre of the plum
slices and used for this assay. The force and height values obtained were
used to calculate the Hencky stress (σ H ) and strain (εH ) parameters,
according to Eqs. (5) and (6), while the stress (σ F ) and strain (εF ) at
failure were determined from the peak of the stress–strain curve (Per­
eira, Ferrari, Mastrantonio, Rodrigues, & Hubinger, 2006).
σ H = F(t)/A(t)
εH = ln(H(t) / H0 )
where F(t), A(t) and H(t) are, respectively, the force, product area and
height, at time t, and H0 is the initial product height. Six plum slices from
each treatment were used for the analysis of mechanical properties.
Measurements were taken from both sides (skin and flesh surfaces) of
each piece of fruit.
2.9. Determination of inulin and glycerol uptake
Prior to analysis, the samples obtained after conventional drying
were well-homogenized, using an Omni mixer homogenizer (Ivan Soe­
vall, Norwalk, CT, USA). For the inulin and glycerol extraction, 25 mL of
pure water were added to approximately 0.5 g of homogenized samples.
The extraction procedure was carried out in an ultrasonic bath (P-
Selecta Model 516, Barcelona, Spain), at a frequency of 35 kHz, at 70 ◦ C,
for 15 min. The supernatant was then recovered, and a second extraction
was performed on the sample residue. The two extractions were then
combined and diluted to a final volume of 50 mL. They were then
filtered through a 0.45 μm nylon filter (Agilent Technologies) before
injection into a HPLC system (Pencheva, Petkova, & Denev, 2012, pp.
339–344).
The inulin and glycerol analyses were performed by using an Agilent
1200 series HPLC system (Agilent Technologies, Santa Clara, CA)
equipped with a refractive index detector. Separation was achieved in a
Rezex ROA-Organic Acid column (H+ (8%), 300 × 7.8 mm) at a tem­
perature of 70 ◦ C. The refractive index detector was heated at 40 ◦ C. The
sample volume injection was 10 μL and the mobile phase of Milli-Q
water at a flow rate of 1 mL min− 1 was used. Quantitation was carried
out through external calibration method, using inulin and glycerol as
standards. The analyses of the inulin and glycerol contents were
repeated three times.
2.10. Experimental design, process optimization and statistical analysis
The response surface methodology (RSM) was applied to estimate
the main effects of the independent variables: water (W), glycerol (Gly)
and inulin content (Inu), during the dehydration process. The responses
(dependent variables) WL, WR and SG were measured after OD; INU,
GLY, ΔE* and the mechanical properties (σF and ƐF) were measured
after the CD of the plums, while aw was measured after OD and CD. A
Box-Behnken Design, involving three independent variables at three
different levels, was used to design the experimental data. The complete
design consisted of 15 experimental points, with three replications of the
central points. The experiments were conducted randomly in order to
LWT 157 (2022) 113092
minimize the potential effects of unexplained variability in the observed
(4)
responses resulting from external factors. The design variables selected
for this study, and their real and coded levels, are provided in Table 1. A
second order polynomial equation was fitted to the experimental data
corresponding to each dependent variable, as follows (Eq. (7)):
∑
3 ∑
3 ∑
2 ∑
3
Yk = βk0 + βki χ i + βkii χ 2i + βkij χ i χ j (7)
i=1 i=1 i=1 j=i+1
where Yk is the response variable; χ i and χ j represent the independent
variables; βk0 is a constant term, and βki , βkii and βkij are, respectively, the
linear, quadratic and interaction regression coefficients.
The mathematical models were evaluated for each response by
means of multiple linear regression analysis, which involved linear,
quadratic, and interaction terms of the independent factors. An analysis
of variance was conducted to determine the significant effects of the
process variables in each response. Significance was judged by deter­
mining the probability of the F-statistic calculated from the data being
less than 5%. The accuracy of the model was tested using the p-value,
(5) coefficient of correlations (R2 , adjusted R2 and predicted R2 ), and lack of
fit test. Three-dimensional plots were generated by varying two inde­
(6) pendent variables while holding the value of a third constant.
The osmotic process condition was optimized using the desirability
function (Derringer & Suich, 1980; Myers, Douglas, Montgomery, &
Anderson-Cook, 2009). The general approach to analysing the desir­
ability function involves the transformation of each estimated response,
variable Yi, to a desirability value, di , where 0 ≤ di ≤ 1. The transformed
response, di , can have many different shapes. A zero response represents
a completely undesirable response, whereas a response of one represents
the most desirable response. The overall desirability combines the di , of
several responses using the geometric mean for simultaneous optimi­
zation of the responses (Eq. (8)):
/
1
(8)
n
D = (d1 ∗d2 ∗d3 ∗…∗dn )
where di indicates the desirability of the response and n is the number of
responses in the measure. In the present study, a desirability function
was developed to maximize WL, WR and INU, and minimize GLY.
Response surface methodology was applied to the experimental data
using Design Expert program version 12.0 (Statease Inc., Minneapolis,
USA, trial version).
2.11. Statistical analysis
Total colour change (ΔE*), Hencky stress (σH ) and strain (εH ) pa­
rameters are expressed as means ± standard deviation and were ana­
lysed using a one-way analysis of variance (ANOVA). The degree of
significance was set at p < 0.05, Tukey’s Test. Normality was checked
prior to the ANOVA test through a Kolmogorov-Smirnov test. For sta­
tistical studies SPSS 20.0 software was used (SSPS Inc., Chicago, IL,
USA).
3. Results and discussion
The experimental data are shown in Tables 2 and 4. The regression
equations describing the effects of the process variables on the WL, WR,
SG, INU, GLY and aw responses after osmotic dehydration (awO.D. ) and
after conventional drying (awC.D. ), are shown in Table 3. The significant
terms (p < 0.05) were used to propose models for each response, without
damaging the model hierarchy. These models were then tested for ad­
equacy and fitness by analysis of variance (ANOVA). The response sur­
face plots were generated to visualize the combined effect of two
variables on a particular response.
3
I. Palacios Romero et al. LWT 157 (2022) 113092

Table 2 where W, Gly and Inu respectively refer to the water, glycerol and inulin
Results of experimental design for WL, WR, SG, INU, GLY, awO.D. and awC.D. .
contents (g).
un Responses The magnitude of the β values (Table 3) indicated that, at linear
#
WL WR SG INU (mg/ GLY (mg/ aw O.D. aw C.D. level, the most significant variable for WL and WR was Inu, follow by Gly
(%) (%) (%) g) g) (p < 0.01) with a positive effect. At quadratic level, all terms were
1 23.73 22.58 1.15 130.10 686.34 0.949 0.693 significant (p < 0.01), with increasing effects of Inu on WL and WR. A
2 21.11 19.26 1.85 127.86 673.73 0.953 0.717 positive and significant (p < 0.05) interaction effect (p < 0.05) between
3 24.81 22.84 1.96 81.36 733.69 0.937 0.652 W and Gly was also detected for WL and WR responses.
4 25.18 24.21 0.98 67.13 691.42 0.938 0.688
The model fitted to SG showed a low value for the determination
5 23.09 21.51 1.58 50.99 538.43 0.944 0.701
6 22.43 21.12 1.30 45.50 479.29 0.947 0.700 coefficient (R2 = 0.78); this was not in agreement with the predicted R2
7 31.66 30.59 1.07 85.90 418.38 0.945 0.698 (= 0.114) and showed a high value in the variation coefficient (%CV).
8 28.58 27.57 1.01 68.66 403.61 0.949 0.640 This model was there considered unsuitable for the SG response. In this
9 22.30 20.89 1.41 62.73 456.96 0.947 0.705 case, only the lineal term of Inu and the interaction term of W-Gly were
10 24.17 22.18 1.98 46.11 498.40 0.934 0.661
11 28.66 27.66 1.01 125.66 362.76 0.954 0.724
significant (p < 0.05) for SG (Table 3). It was possible to observe a
12 30.37 30.11 0.26 58.25 453.12 0.943 0.648 negative influence of Inu on SG; this indicated that an increase in the
13 26.77 25.62 1.16 67.92 455.92 0.944 0.697 inulin content of the osmotic solution led to a decrease in the fruit solid
14 26.30 24.56 1.74 61.50 446.70 0.941 0.651 uptake (Fig. 1).
15 26.94 25.67 1.27 55.20 483.53 0.943 0.655
Fig. 2a and b shows the response surface plots for WL and WR in
relation to Inu-Gly content with the water content fixed at a constant
3.1. Water loss, weight reduction and solid gain value (500 g). When the Inu concentration was increased to a to a fixed
Gly value, a continuous increase in WL and WR was observed. The os­
As shown in Table 3, the models developed for WL and WR after motic gradient between the intracellular fluid and hypertonic solution
osmotic dehydration were statistically significant (p < 0.001), with no encouraged mass transfer processes (diffusion of water and solid mole­
significant lack of fit (p > 0.05), and they presented high values for the cules) from the samples to the osmotic medium; this occurred until os­
determination coefficient (R2 >0.98). All of this implied that the fitted motic equilibrium was reached. An increase in water removal can
models were appropriate for predicting these responses. In all cases, the therefore be obtained by enhancing the osmotic force of the medium by
determination coefficient (R2 ) and the predicted R2 were in reasonable increasing the solute concentration. Similar findings were reported by
agreement with the adjusted R2 . Chiu, Tham, and Lee (2017), Vieira, Pereira, and Hubinger (2012) and
The codified second order polynomial models for WL and WR are Yadav, Yadav, and Jatain (2012), who also observed an increase in WL
described by Eqs. (9) and (10). with an increase in solute concentration. An initial rise in WL and WR
was observed as the Gly increased for a fixed level of Inu. Even so, from a
WL (%) = 26.67 − 0.75⋅W + 1.09⋅Gly + 3.41⋅Inu + 0.75⋅W⋅Gly − 1.45⋅W 2 certain level of Gly, this trend started to decline and had a progressively
− 1.52⋅Gly2 + 1.22⋅Inu2 smaller influence on WL and WR. Similar results were observed by
Kowalska et al. (2017), who reported that using a combination of sol­
(9)
utes, including sucrose and inulin, led to a higher level of WL compared
WR (%) = 25.28 − 0.67⋅W + 1.12⋅Gly + 3.78⋅Inu + 1.17⋅W⋅Gly − 1.54⋅W 2 to solutions consisting of a single solute.
As previously mentioned, the results showed a downward trend in SG
− 1.53⋅Gly2 + 1.45⋅Inu2 at higher Inu concentrations when compared to concentrated Gly solu­
(10) tions (Fig. 1). This was consistent with the observations of Kowalska

Table 3
Regression coefficients of predicted models for the WL, WR, INU, GLY, awO.D. and.awC.D.
Factor Regression coefficients

WL WR SG INU GLY aw O.D. aw C.D.

β0 (intercept) 26.67 25.28 1.32 61.54 462.05 0.944 0.072

β1 (water) − 0.75* − 0.67* − 0.08 − 4.90 − 16.10 0.001 0.988
β2 (glycerol) 1.09** 1.12** − 0.03 − 24.19*** 24.61* − 0.006*** 0.014*
β3 (inulin) 3.41*** 3.78*** − 0.37** 16.64*** − 41.90** 0.002* 0.418
β12 0.75* 1.17** − 0.42* − 3.00 − 7.42 – –
β13 − 0.61 − 0.66 0.05 − 2.94 11.09 – –
β23 − 0.04 0.29 − 0.33 − 12.70* 12.23 – –
β11 − 1.45** − 1.54** – 14.83** 125.68*** – –
β22 − 1.52** − 1.53** – 25.25*** 108.56*** – –
β33 1.22** 1.45** – − 13.60** − 127.80*** – –
Model p-value 0,00020 0,00012 0,00140 0,00067 0,00013 0,00003 0,07245
R2 0.9896 0.9915 0.7787 0.9831 0.9912 0.8747 0.4564
Adjusted R2 0.9710 0.9761 0.6128 0.9526 0.9753 0.8405 0.3081
Predicted R2 0.8564 0.9289 0.1141 0.8220 0.9104 0.7602 0.0132
Lack of fit p-value 0.2255 0.7060 0.6421 0.5340 0.5628 0.3861 0.6745
C.V. % 2.06 2.16 21.74 8.42 3.59 0.24 3.39

Lack of fit is not significant al p > 0.05.

*p < 0.05.
**p < 0.01.
***p < 0.001.

4
I. Palacios Romero et al.
et al. (2017), who also noted lower SG values in solutions consisting
exclusively of inulin, compared to those with a higher proportion of
sucrose. They observed that osmotic agents with a high molecular
weight produced higher levels of WL and lower levels of SG compared to
other osmotic agents of a lower molecular weight, such as sucrose. This
may be due to the low diffusivity of inulin and therefore its reduced
ability to penetrate tissues (Kowalska, Lenart, & Leszczyk, 2008). As the
osmotic substance concentration increases, a solute-barrier layer is
formed at the surface of the food material. This facilitates water removal
and reduces the loss of solutes and solid gain during the process (Tortoe,
INU (mg / g) = 61.54 − 4.90 ⋅ W − 24.19 ⋅ Gly + 16.64 ⋅ Inu − 12.70 ⋅ Gly ⋅ Inu + 14.83 ⋅ W 2 + 25.25 ⋅ Gly2 − 13.60⋅Inu2
GLY (mg / g) = 462.05 − 16.10 ⋅ W + 24.61 ⋅ Gly − 41.90 ⋅ Inu + 125.68 ⋅ W 2 + 108.56 ⋅ Gly2 − 127.80⋅Inu2
2010). This may be due to a variation in the driving force behind solu­
tions with the same ponderable concentration but which differ in the
molecular weight of the osmotic agent. The size and distribution of the
osmotic substances present in a mixed solution which includes such
substances as glycerol and inulin determine the mass transfer between
the fruit and the osmotic solution (Kowalska et al., 2017).
The ranges of WL and WR values calculated from Eqs. (1) and (2),
21.11–31.66% for WL and 19.26–30.59% for WR (Table 2), are similar
to results observed by other authors with different osmotic agents
(El-Aouar, Moreira Azoubel, Lucena Barbosa, & Xidieh Murr, 2006;
Filho et al., 2015; Maldonado et al., 2020). Nevertheless, the SG values
obtained for all experiments are in the range 0.26–1.28% (Table 2);
these results are lower than those found by other authors. This may be
due to the larger size of the inulin molecule than other osmotic agents
like sucrose, corn syrup and fructo-oligosaccharides (FOS) (El-Aouar
et al., 2006; Maldonado et al., 2020) used in the osmotic solution.
Furthermore, there is a relationship between WL, WR and SG with
type and concentration of osmotic solution, being this parameters
dependent of force osmotic driving at the working conditions.
Fig. 1. Response surface and contour plots for SG as a function of Inu and Gly
(at a constant proportion of W, 500 g).
5
LWT 157 (2022) 113092
3.2. Inulin and glycerol uptake
As shown in Table 3, the models developed for INU and GLY were
significant (p < 0.001) and lack of fit was not significant (p < 0.05).
These models also presented high values for the determination coeffi­
cient (R2 >0.98); this again confirmed that the models were appropriate
for predicting these responses. The determination coefficient (R2 ) and
the predicted R2 were in reasonable agreement with the adjusted R2 . The
regression coefficients of INU and GLY as well as the different terms of
the process variables are shown in Table 3.
(11)
(12)
The codified second order polynomial models are described by Eqs.
(11) and (12).
where, INU and GLY are inulin and glycerol uptake (mg/g), respectively,
and W, Gly and Inu are, respectively, the coded water, glycerol and
inulin content (g).
With respect to INU, the magnitude of the β values indicated that INU
was negatively affected by Gly content and positively affected by Inu
content, with both exhibiting a notable lineal effect (p < 0.001). The
quadratic terms significantly influenced INU (p < 0.01) during the os­
motic dehydration process and had an increasing effect on INU; the only
exception was Inu content term, which had a negative effect. The only
significant interaction effect observed (p < 0.05) was between Gly and
Inu content, with a decreasing effect on INU.
Unlike INU, the magnitude of β values (Table 3) obtained for GLY
indicates that it was mainly affected by Inu, followed by Gly, with both
exhibiting a significative lineal effect (p < 0.05). In quadratic terms, all
the different terms were found to exert a high significant influence (p <
0.001). However, the overall effect of the interactive terms on GLY was
not significant (p > 0.05). At the linear and quadratic levels, it was
possible to observe an intense negative influence of Inu content on the
GLY rate, followed by the significant positive effect of the Gly content.
Fig. 2c and d shows the response surface plots for INU and GLY in
relation to Inu-Gly concentration, while W was fixed at a constant value
(500 g). Fig. 2c shows a pronounced increase in INU with an increase in
Inu at a lower Gly proportion. However, as the Gly level in the osmotic
solution increased, the INU values exhibited a strong decrease. On the
other hand, and as shown in Fig. 2d, an increase in Inu produced an
initial increase in GLY values until a certain level, beyond which the Gly
gain began to decrease. This phenomenon could be explained by the
formation of a gel, promoted by an increase in the inulin concentration
in the presence of glycerol; this could have caused difficulties in the
mobility of glycerol (Kim, Faqih, & Wang, 2001). The minimum GLY
content was obtained at high levels of Inu (100 g) and low levels of Gly
(200 g).
3.3. Water activity
In contrast to the other responses, the independent variables only
affected water activity after osmotic dehydration (awO.D. ) and did so in a
linear manner. Table 3 shows that this model was significant (p < 0.001)
and that lack of fit was not significant (p < 0.05). It also shows high
values of the determination coefficient (R2 >0.85); this confirms that the
models were appropriate for predicting water activity. The determina­
tion coefficient (R2 ) and the predicted R2 were in reasonable agreement
I. Palacios Romero et al.
Fig. 2. Response surface and contour plots for (a) WL, (b) WR, (c) INU and (d) GLY, as a function of Inu and Gly (at a constant proportion of W, 500 g).
with the adjusted R2 . With respect to water activity after conventional
drying (awC.D. ), the analysis of variance produced low values for the
determination coefficients (R2 ≤ 0.50). This model was therefore not
considered predictive for awC.D. response.
The magnitude of the coefficients (Table 3) indicates that awO.D. was
mainly affected by the Gly (p < 0.001), followed by the Inu (p < 0.05).
The Gly showed a negative influence on awO.D. , while the Inu seemed to
have a significant positive effect. Fig. 3 shows a notable reduction in
awO.D. associated with the increase in Gly. In contrast, a rise in Inu
favoured an increase in awO.D. .
The water activity values obtained after osmotic dehydration awO.D.
are high (0.934–0.954) (Table 2) in accordance with others authors
(Dermesonlouoglou, Giannakourou, & Taoukis, 2007; El-Aouar et al.,
2006). This explains that the osmotic drying is most often applied as a
pretreatment before conventional drying as it improves the quality
during storage, reduces the total amount of energy for other subsequent
processes to osmotic drying and achieves the diffusion of the dissolved
substance from the osmotic solution into the tissue (Radojcin et al.,
2021).
3.4. Colour and mechanical properties
The values of ΔE*, σF and εF at failure of plums subjected to different
OD conditions are shown in Table 4. The ANOVA showed that the fitted
6
LWT 157 (2022) 113092
models for skin and flesh ΔE*, σ F and εF at failure exhibited a significant
lack of fit and low values for the determination coefficients (R2 ≤ 0.80)
(data not shown). This implies that the fitted models were not suitable
for describing the experimental data and not appropriate for predicting
these responses either. As a result, the statistical models were not
considered for predicting quality parameters.
Although significant differences were found between the values ob­
tained for ΔE*, σF and εF at failure (Table 4), no correlation was found
with the composition of the osmotic solution. These differences can be
explained by the variability of the initial fruit.
3.5. Process optimization
The results obtained with this experimental design showed that the
fitted models for WL, WR, INU and GLY were suitable for describing the
experimental data. In contrast, the models obtained for aw after OD were
not considered for response prediction. To optimize the dehydration
process, a desirability function was performed for maximum values of
WL, WR and INU and minimum values of GLY. The optimum operating
conditions for W, Gly and Inu were 522 g, 219 g and 100 g, respectively,
according to their respective desirability preferences (Table 5).
Maximum WL, WR and INU and minimum GLY were obtained under
these conditions, respectively producing predicted values of 30%, 29%,
119 mg/g and 373 mg/g for dehydrated plum (Table 5). The overall
I. Palacios Romero et al. LWT 157 (2022) 113092

Table 5
Optimization criteria for different factors (W, Gly and Inu) and responses (WL,
WR, INU and GLY) for optimum conditions.
Desired Lower Upper Importance Solution
goal limit limit

W(g) In range 500 600 3 522

Gly (g) In range 200 400 3 219
Inu (g) In range 50 75 3 100
WL (%) Maximize 21.11 31.66 3 30
WR (%) Maximize 19.26 30.59 3 29
INU (mg/ Maximize 45.50 130.10 3 119
g)
GLY (mg/ Minimize 362.76 733.69 3 373
g)

desirability obtained was 0.89. Under these optimal conditions, the

experimental values were not statistically different (p > 0.05) from
those predicted. This indicated that the models were able to predict
responses and provide satisfactory results.
There is no safety concern regarding the use of glycerol (E 422) as a
food additive and thus, there is no need for a numerical acceptable daily
intake (ADI). An ADI without an explicit indication of the upper limit of
intake (“ADI not specified”) may be assigned to substances of very low
toxicity, especially those that are food constituents or that may be
considered as foods or normal metabolites in man (Mortensen et al.,
Fig. 3. Response surface and contour plots for aw as a function of Inu and Gly 2017).
(at a constant proportion of W, 500 g). Calvo Magro, Sánchez Iñiguez, Palacios Romero, Pérez Corcho, and
Rodríguez Gómez (2019) studied the organoleptic properties of the os­
motic dehydrated plums using glycerol and inulin. The consumer pan­
Table 4
elists were asked to evaluate the characteristics of plums, including
Results of experimental design for ΔE*, σF and ƐF.
appearance, colour, texture, sweet and fruity flavour and overall
Run Responses
acceptability. Sensory analysis of the descriptive parameters showed
#
Skin Flesh ratings of 8 (0–10 scale) except for sweetness, where a rating above 5
ΔE* σF (N/ ƐF ΔE* σF (N/ ƐF was achieved.
mm2) mm2)

1 35.79 ± 0.52 ± 73.17 ± 6.54 ± 1.72 ± 79.79 ± 4. Conclusions

0.83 0.05 5.72 0.89 0.28 8.22
2 36.39 ± 0.51 ± 80.31 ± 9.19 ± 1.40 ± 81.45 ± Combining a Box-Behnken Design and Response Surface Methodol­
1.24 0.08 6.16 0.60 0.39 6.49 ogy provided an effective way to determine the optimum OD conditions
3 35.88 ± 0.49 79.06 8.31 ± 1.46 ± 77.13
for ‘Sun Gold’ plums. The results revealed that the models developed
± ± ±
1.90 0.10 11.20 1.06 0.27 8.12
4 35.78 ± 0.59 ± 85.37 ± 7.94 ± 1.56 ± 85.57 ± were suitable for describing the experimental values of WL, WR, INU
2.13 0.07 3.61 1.16 0.43 4.60 and GLY. Subsequent process optimization through the desirability
5 36.00 ± 0.50 ± 78.55 ± 8.87 ± 0.93 ± 77.29 ± function showed that the optimal composition of the osmotic solution
1.31 0.12 7.28 1.56 0.15 5.54
for the dehydration of plums was: 522 g of W, 219 g of Gly and 100 g of
6 36.43 ± 0.53 ± 77.80 ± 7.92 ± 1.34 ± 78.32 ±
0.65 0.12 6.24 1.12 0.35 3.42 Inu. Under these optimal conditions, we achieved WL, WR, INU and GLY
7 35.67 ± 0.70 ± 80.20 ± 7.50 ± 1.56 ± 84.87 ± values of 30% and 29%, and 119 mg/g and 373 mg/g, respectively. We
0.95 0.21 9.17 0.56 0.43 6.29 can therefore say that the osmotic dehydration of ‘Sun Gold’ plums, as a
8 36.09 ± 1.38 ± 89.15 ± 7.86 ± 3.39 ± 82.05 ± treatment prior to conventional drying, is effective since it helps to
1.54 0.30 6.02 0.83 0.70 3.26
9 36.54 ± 0.47 ± 78.68 ± 9.06 ± 1.36 ± 82.47 ±
reduce water content yet allows us to obtain products enriched in inulin.
1.54 0.08 5.09 1.60 0.54 5.46
10 37.47 ± 1.25 ± 79.88 ± 7.49 ± 0.67 ± 76.88 ± Funding sources
1.36 0.12 5.62 1.21 0.12 7.86
11 37.58 ± 1.05 77.13 8.85 ± 2.78 ± 85.45
± ± ±
This work was supported by the Junta de Extremadura and FEDER
0.45 0.07 10.24 0.87 0.55 6.56
12 37.01 ± 0.65 ± 83.93 ± 8.23 ± 2.73 ± 85.85 ± (projects V INTERREG-INNOACE “Open and smart innovation in the
1.09 0.11 2.91 0.66 0.64 4.48 EUROACE” (POCTEP, 2014–2020), and AGA002-18192).
13 37.31 ± 0.46 ± 71.88 ± 7.80 ± 0.85 ± 81.62 ±
0.73 0.03 6.61 0.96 0.16 3.50 Declaration of interests
14 36.26 ± 0.83 ± 85.63 ± 7.46 ± 1.66 ± 79.39 ±
1.05 0.10 6.84 1.84 0.4 3.75
15 36.72 ± 0.80 ± 86.11 ± 7.50 ± 1.70 ± 81.49 ± The authors declare that they have no known competing financial
0.62 0.19 16.19 1.05 0.51 3.57 interests or personal relationships that could have appeared to influence
the work reported in this paper.

7
I. Palacios Romero et al.
CRediT authorship contribution statement
Irene Palacios Romero: Investigation, Experimental Design,
Methodology, Formal analysis, Writing – original draft. María José
Rodríguez Gómez: Investigation, Experimental Design, Writing – re­
view & editing. Francisco Manuel Sánchez Iñiguez: Investigation,
Experimental Design, Methodology, Formal analysis, Writing – review &
editing. Patricia Calvo Magro: Funding acquisition, Investigation,
Experimental Design, Supervision, Writing – original draft, Writing –
review & editing.
References
Abed, S. M., Ali, A. H., Noman, A., & Bakry, A. M. (2016). Inulin as prebiotics and its
applications in food industry and human health; A review. International Journal of
Agriculture Innovations and Research, 5(1), 2319–1473.
Calvo Magro, P., Sánchez Iñiguez, F. M., Palacios Romero, I., Pérez Corcho, J. T., &
Rodríguez Gómez, M. J. (2019). Valoración sensorial y grado de aceptación de nuevos
deshidratados de ciruela. León, España: X Congreso Nacional CyTA CESIA.
Chiu, M. T., Tham, H. J., & Lee, J. S. (2017). Optimization of osmotic dehydration of
Terung Asam (Solanum lasiocarpum dunal). Journal of Food Science & Technology, 54
(10), 3327–3337. https://doi.org/10.1007/s13197-017-2785-3
Dermesonlouoglou, E. K., Giannakourou, M. C., & Taoukis, P. (2007). Stability of
dehydrofrozen tomatoes pretreated with alternative osmotic solutes. Journal of Food
Engineering, 78, 272–280. https://doi:10.1016/j.jfoodeng.2005.09.026.
Derringer, G., & Suich, R. (1980). Simultaneous optimization of several response
variables. Journal of Quality Technology, 12(4), 214–219. https://doi.org/10.1080/
00224065.1980.11980968
El-Aouar, A. A., Moreira Azoubel, P., Lucena Barbosa, J., & Xidieh Murr, F. E. (2006).
Influence of the osmotic agent on the osmotic dehydration of papaya (Carica papaya
L.). Journal of Food Engineering, 75, 267–274.
Filho, R. S. F., Gusmao, R. P., Silva, W. P., Gomes, J. P., Filho, E. V. C., & El-Aouar, A. A.
(2015). Osmotic dehydration of pineapple stems in hypertonic sucrose solutions.
Agricultural Sciences, 6, 916–924.
Jiménez-Hernández, J., Estrada-Bahena, E. B., Maldonado-Astudillo, Y. I., Talavera-
Mendoza, Ó., Arámbula-Villa, G., Azuara, E., et al. (2017). Osmotic dehydration of
mango with impregnation of inulin and piquin-pepper oleoresin. Lebensmittel-
Wissenschaft und -Technologie- Food Science and Technology, 79, 609–615. https://doi.
org/10.1016/j.lwt.2016.11.016
Kim, Y., Faqih, M. N., & Wang, S. S. (2001). Factors affecting gel formation of inulin.
Carbohydrate Polymers, 46(2), 135–145. https://doi.org/10.1016/S0144-8617(00)
00296-4
Kowalska, H., Lenart, A., & Leszczyk, D. (2008). The effect of blanching and freezing on
osmotic dehydration of pumpkin. Journal of Food Engineering, 86(1), 30–38. https://
doi.org/10.1016/j.jfoodeng.2007.09.006
Kowalska, H., Marzec, A., Kowalska, J., Ciurzyńska, A., Czajkowska, K., Cichowska, J.,
et al. (2017). Osmotic dehydration of Honeoye strawberries in solutions enriched
with natural bioactive molecules. Lebensmittel-Wissenschaft und -Technologie- Food
Science and Technology, 85, 500–505. https://doi.org/10.1016/j.lwt.2017.03.044
Landim, A. P. M., Barbosa, M. I. M. J., & Júnior, J. L. B. (2016). Influence of osmotic
dehydration on bioactive compounds, antioxidant capacity, color and texture of
fruits and vegetables: A review. Ciência Rural, 46(10), 1714–1722. https://doi.org/
10.1590/0103-8478cr20150534
Lemus-Mondaca, R., Noma, S., Igura, N., Shimoda, M., & Pérez-Won, M. (2014). Kinetic
modeling and mass diffusivities during osmotic treatment of red Abalone (Haliotis
rufescens) slices. Journal of Food Processing and Preservation, 39(6), 1889–1897.
https://doi.org/10.1111/jfpp.12426
Lewicki, P. P. (2006). Design of hot air drying for better foods. Trends in Food Science &
Technology, 17(4), 153–163. https://doi.org/10.1016/j.tifs.2005.10.012
Maldonado, R. R., Mendes Pedreira, A. J., Cristianini, L. B., Guidi, M. F., Oliveira
Capato, M., Ávila, P. F., et al. (2020). Application of soluble fibres in the osmotic
LWT 157 (2022) 113092
dehydration of pineapples and reuse of effluent in a beverage fermented by water
kefir. Food Science and Technology, 132, Article 109819.
Mortensen, A., Aguilar, F., Crebelli, R., Di Domenico, A., Dusemund, B., Frutos, M. J.,
et al. (2017). Re-evaluation of glycerol (E 422) as a food additive. EFSA Journal, 15
(3), 4720. https://doi.org/10.2903/j.efsa.2017.4720, 64 pp.
Myers, R. H., Montgomery, D. C., & Anderson-Cook, C. M. (2009). In W. J (Ed.), Response
surface methodology: Process and product optimization using designed experiments (3rd
ed.) Sons.
Nagai, L. Y., Santos, A. B., Faria, F. A., Boscolo, M., & Mauro, M. A. (2015). Osmotic
dehydration of mango with ascorbic acid impregnation: Influence of process
variables. Journal of Food Processing and Preservation, 39(4), 384–393. https://doi.
org/10.1111/jfpp.12243
Pencheva, D. N., Petkova, N. T. R., & Denev, P. P. (2012). Determination of inulin in Dough
products. Scientific Works of UFT. https://doi.org/10.13140/RG.2.1.4174.1848. LІX-
2012.
Pereira, L. M., Ferrari, C. C., Mastrantonio, S. D. S., Rodrigues, A. C. C., &
Hubinger, M. D. (2006). Kinetic aspects, texture, and color evaluation of some
tropical fruits during osmotic dehydration. Drying Technology, 24(4), 475–484.
https://doi.org/10.1080/07373930600611968
Porat, R., Lichter, A., Terry, L. A., Harker, R., & Buzby, J. (2018). Postharvest losses of
fruit and vegetables during retail and in consumers’ homes: Quantifications, causes,
and means of prevention. Postharvest Biology and Technology, 139, 135–149. https://
doi.org/10.1016/j.postharvbio.2017.11.019. February.
Radojcin, M., Pavkov, I., Bursac, D., Putnik, P., Wiktor, A., Stamenkovic, Z., et al. (2021).
Effect of selected drying methods and emerging drying intensification technologies
on the quality of dried fruit: A review. Processes, 9, 132. https://doi.org/10.3390/
pr9010132
Commission Regulation (EU) No 1130/2011 of 11 November 2011 amending Annex III
to Regulation (EC) No 1333/2008 of the European Parliament and of the Council on
food additives by establishing a Union list of food additives approved for use in food
additives, food enzymes, food flavourings and nutrients.
Regulation (EC) No 1924/2006 of the European Parliament and of the Council of 20
December 2006 on nutrition and health claims made on foods.
Roberfroid, M. B. (2000). Chicory fructooligosaccharides and the gastrointestinal Tract.
Nutrition, 16, 677–679.
Roussos, P. A., Efstathios, N., Intidhar, B., Denaxa, N. K., & Tsafouros, A. (2015). Plum
(Prunus domestica L. And P. Salicina Lindl.). In Nutritional composition of fruit
cultivars. Elsevier Inc. https://doi.org/10.1016/B978-0-12-408117-8.00026-X.
Sahamishirazi, S., Moehring, J., Claupein, W., & Graeff-Hoenninger, S. (2017). Quality
assessment of 178 cultivars of plum regarding phenolic, anthocyanin and sugar
content. Food Chemistry, 214, 694–701. https://doi.org/10.1016/j.
foodchem.2016.07.070
Salazar-López, E. I., Jiménez, M., Salazar, R., & Azuara, E. (2015). Incorporation of
microcapsules in pineapple intercellular tissue using osmotic dehydration and
microencapsulation method. Food and Bioprocess Technology, 8(8), 1699–1706.
https://doi.org/10.1007/s11947-015-1534-8
Sritongtae, B., Mahawanich, T., & Duangmal, K. (2011). Drying of osmosed cantaloupe:
Effect of polyols on drying and water mobility. Drying Technology, 29(5), 527–535.
https://doi.org/10.1080/07373937.2010.513615
Tortoe, C. (2010). A review of osmodehydration for food industry. African Journal of Food
Science, 4(6), 303–324. https://doi.org/10.5897/AJFS.9000007
Vieira, G. S., Pereira, L. M., & Hubinger, M. D. (2012). Optimisation of osmotic
dehydration process of guavas by response surface methodology and desirability
function. International Journal of Food Science and Technology, 47(1), 132–140.
https://doi.org/10.1111/j.1365-2621.2011.02818.x
Wojdyło, A., Figiel, A., Lech, K., Nowicka, P., & Oszmiański, J. (2014). Effect of
convective and vacuum-microwave drying on the bioactive compounds, color, and
antioxidant capacity of sour cherries. Food and Bioprocess Technology, 7(3), 829–841.
https://doi.org/10.1007/s11947-013-1130-8
Yadav, A. K., & Singh, S. V. (2014). Osmotic dehydration of fruits and vegetables: A
review. Journal of Food Science & Technology, 51(9), 1654–1673. https://doi.org/
10.1007/s13197-012-0659-2
Yadav, B. S., Yadav, R. B., & Jatain, M. (2012). Optimization of osmotic dehydration
conditions of peach. Journal of Food Science & Technology, 49(5), 547–555. https://
doi.org/10.1007/s13197-011-0298-z