Biomass Conversion and Biorefinery

https://doi.org/10.1007/s13399-023-05234-1

ORIGINAL ARTICLE

Production of cornelian cherry (Cornus mas L.) pulp powder

by foam‑mat drying: analysis of physicochemical and antioxidant
properties
Beyza Kaba1 · Yasemin Yıkılkan1 · Hojjat Pashazadeh1,2 · Ali Ali Redha3,4 · Ilkay Koca1

Received: 2 October 2023 / Revised: 1 December 2023 / Accepted: 12 December 2023

© The Author(s) 2023

Abstract
Cornelian cherry (Cornus mas L.) is a rich source of (poly)phenols such as phenolic acids, flavonoids, and anthocyanins that
are known for their bioactivity. This study aimed to enhance the industrial applications of this cherry’s pulp as a potential
functional food ingredient. Foam-mat drying was used to produce cherry powder from cherry pulp. The convective drying
process was performed at different temperatures (50, 60, 70, and 80°C) to study the effect of drying temperature on the physi-
cal properties, flow properties, microstructure, (poly)phenol content, antioxidant properties, and bioaccessibility of foam-
dried cherry pulp, in comparison to freeze-dried sample. Different drying temperatures did not affect color properties. The
highest gloss was determined at high temperatures (70–80°C). According to the Carr index, the fluidity increased between
18 and 22% as the temperature increased. The total phenolic content was higher at elevated temperatures (70–80°C), yet the
anthocyanin content was the highest at 60°C. The flavonoid content was not affected by different drying temperatures, as
well as compared to lyophilized samples. The antioxidant activity was higher in samples dried at elevated temperatures, with
no significant difference in comparison to lyophilized samples. The bioaccessibility experiment showed that the lyophilized
samples had significantly greater bioaccessibility in comparison to the convective dried samples, yet further investigation is
required to understand the differences in bioaccessibility and bioavailability of individual polyphenols. Overall, foam-mat
drying using a convective drying system could be an economic choice to preserve acceptable amounts of phenolics and
antioxidants.

Keywords Drying · Foam-mat drying · Cornelian cherry · Antioxidants · Fruit powder · Fruit pulp

1 Introduction

Cornelian cherry (CC), Cornus mas L., belongs to the fam-

ily of Cornaceae. This tree is native to southern Europe and
* Hojjat Pashazadeh
[email protected] southwest Asia [1]. CC fruits contain high amounts of dif-
ferent reducing sugars and acids. In addition, it is a rich
* Ali Ali Redha
[email protected] source of ascorbic acid (vitamin C) and (poly)phenols such
as anthocyanins. The amount of ascorbic acid present in CC
1
Department of Food Engineering, Faculty of Engineering, fruit was reported to be two times greater than in oranges.
Ondokuz Mayis University, 55139 Samsun, Turkey The amount of anthocyanins present in CC fruit can range
2
Hafızbaba Bitkisel ve Kozmetik Ürünler Pazarlama Gıda between 34 and 292 mg/100 g [2]. A wide range of antho-
Sanayi Tic. Ltd. Şti, Istanbul, Turkey cyanins have been reported in CC fruit including cyanidin-
3
The Department of Public Health and Sport Sciences, 3-glucoside, cyanidin-3-rutinoside, cyanidin-3-galactoside,
University of Exeter Medical School, Faculty of Health delphinidin-3-galactoside, pelargonidin-3-glucoside, and
and Life Sciences, University of Exeter, Exeter EX1 2LU,
UK pelargonidin-3-galactoside [3]. In fact, CC fruits also con-
4 tain other polyphenols such as gallic acid, rutin, resveratrol,
Centre for Nutrition and Food Sciences, Queensland
Alliance for Agriculture and Food Innovation (QAAFI), The chlorogenic acid, and quercetin [2].
University of Queensland, Brisbane, QLD 4072, Australia

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Due to the rich phytochemical content of CC fruits, they is performed is the main factor considered in the study. The
have been reported for their ethnomedicinal applications effect of temperature on the physical properties (color, pH,
[4]. CC fruits, flowers, leaves, and bark have been widely water activity, and percentage dry matter), flow properties
used in Asian folk medicine. They have been used for diar- (bulk density, tap density, Hausner ratio, Carr index, and
rhea, lowering blood sugar, common cold, liver diseases, solubility), microstructure, (poly)phenol content (phenolics,
and weight loss. The CC fruit extracts have cosmetic appli- flavonoids, and anthocyanins), antioxidant properties, and
cations as well and are used as a replacement for synthetic bioaccessibility of foam-dried pulp.
astringents [4].
CC fruits have the potential to become a functional food
ingredient due to their rich phytochemical content and 2 Material and methods
reported benefits. However, despite their valuable pro-health
properties, these fruits are widely used in the food produc- 2.1 Samples
tion industry. Drying these fruits could potentially increase
their applications in the food industry and make them more Fresh CC fruits were purchased from the local market (Sam-
compatible with the development of functional food prod- sun, Turkey) in the summer of 2023. Fruits were washed
ucts. Drying can lower the moisture content of the fruit, with water after the removal of stems and leaves. The fruits
thus preventing microbial spoilage and undesired enzymatic were boiled in steam for 10 min. The seed was removed
changes [5]. Drying can be done by natural and artificial manually, and the fruits were juiced using a commercial
techniques [6]. Today, many artificial drying techniques have juicer. The solid material left over after juicing was blended
been developed that have advantages over natural drying. with distilled water to help remove any remaining juice. The
Few of these developed techniques are used for drying liq- mixture was then sieved through a 500-μm sieve, and the
uid products. Foam-drying, freeze-drying, and spray-drying remaining pulp was collected for the foaming experiment.
techniques are mostly used for drying liquid products [7].
One of the techniques that is used to produce fruit pow-
ders is foam drying. Foam drying is suitable for drying fruits 2.2 Foaming experiment
which are heat-sensitive, have high sugar content, and have a
viscous nature [8]. In the process, the fruit is converted from The foamed CC pulp was prepared by mixing the foaming
liquid to stable foam (by whipping, bubbling, or shaking), agent and foaming stabilizers with the pulp at room tempera-
with the addition of surfactants, and then dried by different ture. The foaming agent used was 10% egg albumen, and the
methods [9]. Advantages of this technique include compat- foaming stabilizers were carboxyl methylcellulose (1.0%)
ibility with most types of juices, fast drying at lower tem- and maltodextrin (MD) (10%). A commercial blender was
peratures, preservation of nutritional quality, easy reconsti- used to form the foam by whipping for 5 min.
tution, and cost-effectiveness to produce easily reconstituted
juice powders. 2.3 Freeze‑drying
So far, many fruits such as cherry [10], kiwi [11], blue-
berry [12], mango [13], dates [14], papaya [15], bitter orange The frozen foam was dried for 48 h (until reaching a con-
[16], raspberry [17], and guava [18] have been successfully stant mass) using a freeze-dryer (Labconco Freezone 12
dried by foam drying. It has been stated that since the total Plus, USA) operating at −80°C and 13 Pa. The freeze-dried
surface area available for drying is increased by foaming samples were turned into fine powder and stored in sealed
the product, the drying time is significantly shortened, aluminum foil bags at −18°C.
and therefore, the fruits are exposed to the heat effect for a
shorter period of time [14]. Foam mat drying has proven to
2.4 Convective drying
be an effective technique for producing fruit powders while
preserving both their physical characteristics and nutritional
The foams were dried with the convective system we used
properties, ensuring originality in the content [13].
in our previous study [19]. In drying, air temperatures were
Although this technique has been widely applied to
set at 50, 60, 70, and 80°C, and the air velocity was 1.0 m/s.
fruits, this technique has not been investigated with many
fruit waste products — such as CC pulp. Thus, the current
study aimed to evaluate the potential of foam drying to uti- 2.5 Foam analysis
lize CC waste (pulp) towards sustainable processing and
production. The developed powder could potentially be a Foam expansion, foam density, and foam stability analy-
functional food ingredient used in the development of other ses were performed on the foam according to previously
products. The temperature at which the foam drying process reported methods [20].

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2.5.1 Foam expansion 2.6.4 pH analysis

The percentage change was determined by measuring the A digital pH meter (ORION 3-Star, USA) was used to meas-
volume before and after foam formation. ure the pH of the pulp and reconstituted CC pulp powder.

2.5.2 Foam density
2.6.5 Moisture ratio
The density was determined by transferring the foam to a
measuring cylinder, determining its volume and weight, and The moisture content of CC foam during the drying process
proportioning it to each other. was determined using the concept of moisture ratio (MR),
represented by the equation:
2.5.3 Foam stability
(Mt − Me)
MR = (1)
The foam was transferred to a measuring tape and left at (Mi − Me)
room temperature for 3 h. Volume reduction was measured In this equation, Mt refers to the moisture content at any
every 30 min. given time during drying, Mi represents the initial moisture
content, and Me represents the equilibrium moisture content
2.6 Properties of fresh and powdered pulps (db) (kg water/kg dry solid). By using the moisture ratio, the
changes in moisture content throughout the drying process
2.6.1 Color can be quantified and analyzed [22].

The color of fresh and powdered pulps was analyzed using a

colorimeter (MiniScan EZ 4500, Reston, VA, USA). 2.7 Drying models
2.6.2 Moisture content In order to select the most suitable drying model that repre-
sents the drying process of the CC foam, drying curves were
The moisture content was determined gravimetrically fitted with 11 thin-layer drying MR models (Table 1). Curve
according to the standard method 934.06 [21]. In this fitting toolbox and Levenberg–Marquardt algorithm were
method, samples were dried to a constant weight under used for data fitting in MATLAB software (R2016d). The
vacuum at 70 °C. fitting quality of the proposed models was assessed based on
different statistical parameters:
2.6.3 Water activity
1. Determination of coefficient (R2):
The water activity (aw) of fresh and powdered pulps was
performed on a water activity meter (AquaLab 4TE), at
25 °C.

Table 1  Mathematical models Model No. Model name Model equation (MR) References
used to evaluate the drying
kinetics of foam-dried cornelian 1 Newton exp(−k·x) [23]
cherry pulp powder
2 Page exp(−k·xn) [24]
3 Henderson ve Pabis a·exp(-k·t) [25]
4 Logarithmic a·exp(−k·x)+b [26]
5 Two-term a·exp(−k·x)+b·exp(−g·x) [25]
6 Two-term exponential a·exp(−k·x)+(1−a)·exp(−k·a·x) [27]
7 Wang ve Singh 1+(a·x)+b·x2 [28]
8 Approximation of diffusion a.exp(−k·x)+(1−a)·exp(−k·b·t) [29, 30]
9 Logistic b/(1+a·exp(k·x)) [31]
10 Midilli a·exp(−k·(xn))+(b·x) [32]
11 Aghabashlo model exp(−k·x/(1+g·x)) [33]

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 Biomass Conversion and Biorefinery

∑ n� �2 ∑ n �
MRExp,i − MRpre − MRExP,i − MRpre,i
�2 samples and attached to a stainless rod with double-bond
2
j j tape. The assembly was then immediately sputtered with a
R =
∑ n� �2 gold/palladium target (60/40) at approximately 10 nm for
MRExp,i − MRpre 2 min using a spray coater powered by a flow of argon and
j
2. Reduced chi-square (χ2): (2) plasma. Images were recorded at 10 kV and 15 kV accelera-
∑ N � �2 tion rates.
MRExP,i − MRpre,i
i=1 (3)
X2 = 2.8.4 Fourier transformed infrared analysis
N−n
3. Root mean square error (RMSE):
An FTIR spectrometer (Perkin Elmer, Spectrum-Two, USA,
�
� n
�∑ � �2
�
� j
MRExP,i − MRpre,i
(4) PEService 35) was used to scan the samples and obtain the
RMSE = spectra of the region 4000 to 400 ­cm-1.
n
The best model describing thin-layer drying characteristics 2.9 Analysis of polyphenol content
of CC foam will have the highest R2 values and lowest values
of χ2 and RMSE [22]. 2.9.1 Extraction

2.8 Characterization of product An amount of 1 g of each powder sample was extracted with

50 mL of 80% methanol by ultrasound-assisted extraction.
2.8.1 Flowability, and bulk and tapped density The samples were kept in an ultrasonic water bath (Soni-
clean™, Thermo Scientific, USA) for 20 min at 30°C with
The flowability of pulp powders is represented by numeri- 100 W power. Then, samples were centrifuged for 15 min
cally calculated Hausner ratio (HR) and Carr index (CI). The and 4000 rpm. The supernatant was collected for total phe-
apparent and tap densities of the powders were measured in nolic content (TPO), total flavonoid content (TFO), and total
other to determine the HR and CI values [34]. Bulk density anthocyanin content (TACN) analysis.
was determined by measuring the volume filled with 1 g of CC
powder per 25-mL graduated cylinder by pouring it from top
2.9.2 Total phenolic content
to bottom. On the other hand, before the volume of the powder
is recorded, the impact intensity is measured after the gradu-
The total phenolic content (TPO) was determined by
ated cylinder containing the powder has been struck 80 times.
the spectrophotometric Folin-Ciocalteu method [35]. A
volume of 150 μL of extract was mixed with 750 μL of 10%
2.8.2 Solubility
Folin-Ciocalteu reagent and vortexed for 1 min. Then, 600
μL of 7.5% ­Na2CO3 solution was added to the mixture. The
The solubility was determined as described by Abbasi and
mixture was vortexed again and incubated at room tem-
Azizpour [10]. For this, 100 mL of distilled water was trans-
perature in the dark for 2 h. Finally, the absorbance was
ferred to a blender jar. Then, an amount of 1 g of CC pulp
measured at 760 nm using a UV/VIS spectrophotometer
powder was added slowly to mixer running at 1500 rpm. After
(LAMBDA™ 365, Perkin Elmer, USA). The TPO was cal-
5 min, the sample was centrifuged at 4300 g for 10 min. An
culated and reported as gallic acid equivalents (GAE); mg
aliquot (25 mL) of the obtained supernatant was transferred
GAE/g dry weight (dw).
into Petri dishes and dried in a 105°C oven for 5 h. The solubil-
ity percentage was calculated according to Eq. (5):
2.9.3 Total flavonoid content
m − m1
Solubility (%) = 2 × 100 (5)
0.25 The total flavonoid content (TF) was determined spectropho-
where m2 is the final mass of the Petri dish containing the ­ lCl3 method [35]. A volume
tometrically according to the A
sample, and m1 is the mass of the empty Petri dish. of 1 mL of extract was mixed with 0.3 mL of 5% N ­ aNO2.
After 5 min, a volume of 0.5 mL of 5% ­AlCl3 was added.
2.8.3 Microstructure After waiting for 6 min, a volume of 0.5 mL of 1 M NaOH
was added and vortexed. Finally, after 10 min, the absorb-
The microstructure of different CC pulp powders was per- ance was measured at 510 nm using a UV/VIS spectropho-
formed using a scanning electron microscope (SEM, JEOL tometer (LAMBDA™ 365, Perkin Elmer, USA). The TF
JSM-7001F). A small sample was briefly taken from the was calculated and reported as quercetin equivalents (QE);
mg QE/g dw).

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Biomass Conversion and Biorefinery

2.9.4 Total anthocyanin content was measured at 593 nm using a UV/VIS spectrophotometer

(LAMBDA™ 365, Perkin Elmer, USA). The FRAP was cal-
The total monomeric anthocyanin (TACN) was determined culated from a calibration curve using ­FeSO4 as a standard,
based on the pH differential method [36]. Extracts were and results were reported as mmol F
­ eSO4 equivalent (ISE)/g
diluted with buffers (pH 1.0 (0.025 M KCl) and 4.5 (0.4 M dw.
­CH3COONa)) and their absorbance was measured at 520 and
700 nm using a UV/VIS spectrophotometer (LAMBDA™ 2.11 Measurement of bioaccessibility
365, Perkin Elmer, USA). TACN was then calculated and
reported as cyanidin-3-glucoside equivalents (CGE); mg In vitro digestion of the samples was performed according
CGE/g dw according to Eq. (6): to a previously published method [37]. A volume of 5 mL of
At × Mw × Df each sample was combined with 20 mL of simulated gastric
TA = (6) fluid containing 1.5 mL of pepsin (3.2 g/L). The pH of the
𝜀×l
mixture was adjusted to 1.7 using HCl (1 M). The mixture
where At = (absorbance at 520 nm – absorbance at 700 nm) was incubated for 2 h at 37°C with continuous shaking. After
pH 1.0 – (absorbance at 520 nm – absorbance at 700 nm) 2 h, the pH of the mixture was adjusted to 7 with NaOH (1
­ w (molecular weight) = 449.2 g/mol for cyanidin-
pH 4.5; M M). A volume of 4 mL bile salt (5 g/L) and 1 mL C ­ aCl2
3-glucoside, Df = dilution factor, l = path length in cm, (0.75 M) were added, followed by 2.5 mL of lipase (4.8
and ϵ (molar extinction coefficient) = 26900 L/mol cm for g/L). The pH of the mixture was adjusted to 7 with NaOH
cyanidin-3-glucoside. (1 M) and incubated for 2 h at 37°C with continuous shak-
ing. After 2 h, an aliquot of each sample was collected and
2.10 Analysis of antioxidant potential centrifuged at 4°C for 15 min at 5000×g. The TPO of super-
natant was determined according to the previous method
2.10.1 DPPH radical scavenging activity (Section 2.9.1.). The bioaccessibility was calculated accord-
ing to the following equation:
The 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scaveng- Bioaccessibility (%) = (Cd∕Cud) × 100 (5)
ing potential of the powders was spectrophotometrically
determined [35]. A volume of 50 μL of extract was mixed where Cd and Cud are the concentrations of the TPO in the
with 1-mL DPPH solution (0.06 mM in 80% methanol). The digested powder sample and the undigested powder sample,
solution was incubated at room temperature in the dark for 1 respectively.
h. Finally, the absorbance of the solutions was measured at
517 nm using a UV/VIS spectrophotometer (LAMBDA™ 2.12 Statistical analysis
365, Perkin Elmer, USA). The radical scavenging activity
was calculated using Eq. (7): All experiments were performed in triplicate. IBM SPSS
AC − AS Statistics V22.0 (International Business Machines (IBM)
DPPH scavening activity = × 100 (7) Corporation, Armonk, NY, USA) software was used for
AC
statistical analysis. The analysis of variance (ANOVA) and
where AC is the absorbance of pure DPPH solution and comparison among means was determined according to
AS is the absorbance of the test sample. The DPPH radi- Duncan’s new multiple range test at 95% confidence level.
cal scavenging activity was calculated from a calibration
curve using Trolox as a standard and results were reported
as mmol Trolox equivalent (TE)/g dw. 3 Results and discussion

2.10.2 Ferric‑reducing antioxidant power 3.1 Properties of CC pulp

Ferric-reducing antioxidant power (FRAP) determination The physicochemical properties of CC pulp were examined
was performed according to the spectrophotometric method before any drying treatment. The pulp had 91.06±1.09%
proposed by Zannou and Koca [35]. A volume of 50 μL of moisture content, 8.00±0.09% total soluble solids, and a
extract was mixed with 950 μL of 950 mM of FRAP solu- pH of 3.70±0.10. Moldovan and David [38] found the pH
tion (comprised of 100 mM acetate buffer, 10 mM F ­ eCl3, value of the CC they used in the study to be 3.12 ± 0.04.
and 10 mM TPTZ (2,4,6-tripyridyl-s-triazine)). The solution This result is similar to ours. Szczepaniak et al. [39] reported
was shaken for 5 min, and the absorbance of the solutions that the soluble solids content of CC juice varied between
10.7 and 19.3%. These differences are thought to be related

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 Biomass Conversion and Biorefinery

to genotype variation. The L*, a*, and b* values of pulp

were 44.29±0.41, 7.94±0.20, and 19.99±0.31, respectively.
Güzel [40] stated that the % dry matter values in cranberry
fruit vary between 14.43 and 27.49, the L* value in color
measurement varies between 25.18 and 33.00, the a value
between 9.74 and 30.26, and the b value between 2.46 and
14.41. Our results are outside these stated ranges. These dif-
ferences in physical properties are thought to be due to the
fact that the fruit may be different in whole and pulp form.
In this study, egg white, maltodextrin, and carboxymethyl
cellulose (10:10:1, w/w) obtained as a result of the prelimi-
nary study were used in a single ratio. The density, stability,
and expansion values of CC foam were found as 0.55±0.01
g/cm 3, 98.68±1.00%, and 67.00±0.50 %, respectively.
Krasaekoopt [41] determined that the optimum concentra-
tion of egg albumin for drying yoghurt with the foam drying
method was 3%. They determined the foam expansion to be
between 67.6 and 70.0%. This result is consistent with our Fig. 1  Drying curves of cornelian cherry foams at different tempera-
findings. Shameena Beegum [42] observed that the protein- tures using convective drying method
based nature of foam stabilizers plays the role of surfactant.
The kinetic stability of the foam balanced its thermodynamic
instability. Additionally, in their study, they obtained the best and 50°C. As a result of the study, Two-term exponential
foam expansion result from sodium caseinate. In our study, and Henderson, which is one of the thin-layer drying mod-
egg albumin gave positive results in terms of expansion, and els of cranberry fruit, determined that it provided the most
its selection was also evaluated in terms of accessibility and appropriate correlation in Pabis models. In another study
cost. Other studies in the literature also used egg albumin to examining the drying kinetics of CC fruit and the degrada-
create foam stability [43]. tion of vitamin C, it was determined that Henderson and
Pabis, modified from thin layer drying models of samples
3.2 Drying kinetics dried at 50, 60, and 70°C, provided the most appropriate
correlation [47].
Increasing the drying temperature resulted in a significant In a study in which foam drying was performed at 65,
decrease in drying time as seen in Fig. 1. This is due to the 75, and 85°C with 0–9% egg white using mango pulp, the
fact that increasing the temperature will result in an increase increase in egg white concentration adversely affected the
in molecular movement, enhancing the removal rate of mois- drying properties. While the optimum ratio was chosen as
ture, which leads to a reduction in the drying time. In the 3% egg white, the Wangh and Singh model was found suit-
foam mat drying method, because of the porous structure, able for thin layer drying models at 65 and 85°C, while the
increasing the drying temperature greatly affects the dry- logarithmic and diffusion models were found suitable for
ing rate. The porous structure of the foam mat allows water 75°C [48]. Azizpour et al. [49] found that the moisture con-
vapor to escape quickly at high drying temperatures, which tent decreased with increasing drying time in the foam dry-
increases the drying rate [10]. Kadam and Balasubramanian ing of shrimp. Among the drying models, they determined
[44] and Abd Karim and Wai [45] reported similar results. that the Midilli model gave the highest R2, the lowest RMSE,
Drying rates were generally in the decreasing rate period. In and X2 values. In our study, it has been determined that the
the foam drying method, the drying rate varies depending on Aghabashlo model, which is one of the thin layer drying
the agents used, the chemical structure of the food, and its models, is the most suitable model for CC pulp foam drying
content [45]. As the water content decreased, a decrease was by giving high R2, low RMSE, and X2 values.
observed in the drying rate occurring in the inner regions of
the foam as the outer layers dried faster. As the surface area 3.3 Physical properties
of the food increases, the dehydration process is easy. The
constants and statistical parameters obtained for the cran- The physicochemical characteristics of CC pulp powder
berry pulp foam are given in Table 2. are given in Table 3 and the powders prepared using foam-
Kaya and Aydin [46] investigated the drying kinetics and mat drying are shown in Fig. 2. The observed L* value of
drying behaviors of CC dried with the help of a convec- powder ranged from 63.15±0.06 to 66.35±1.32, a* value
tive dryer. They were dried in a convective dryer at 30, 40, ranged from 27.46±1.98 to 31.57±0.61, and b* value ranged

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Biomass Conversion and Biorefinery

Table 2  Constants and statistic Model name Drying temperature Statistical parameters
parameters obtained for foam- (°C)
dried cornelian cherry pulp R2 RMSE X2
powder
Newton 50 0.976423 0.044632 0.001992
60 0.935507 0.074625 0.005568
70 0.860296 0.105832 0.011200
80 0.884013 0.106748 0.011395
Page 50 0.985749 0.037480 0.001404
60 0.993742 0.025463 0.000648
70 0.985250 0.037670 0.001419
80 0.999844 0.004510 0.000002
Henderson ve Pabis 50 0.977673 0.046913 0.002200
60 0.944580 0.075779 0.005742
70 0.880350 0.107290 0.011511
80 0.895331 0.117094 0.013711
Logarithmic 50 0.989169 0.035792 0.001281
60 0.992550 0.031061 0.000964
70 0.986095 0.040892 0.001672
80 0.997480 0.022248 0.000494
Two-term 50 0.989444 0.039506 0.001560
60 0.988146 0.045244 0.002047
70 0.988555 0.042838 0.001835
80 0.999961 0.003907 0.000015
Two-term exponential 50 0.987582 0.034987 0.001224
60 0.972574 0.053308 0.002841
70 0.919511 0.087998 0.007743
80 0.934588 0.092566 0.008568
Wang ve Singh 50 0.974024 0.050602 0.002560
60 0.931678 0.084139 0.007079
70 0.903302 0.096452 0.009303
80 0.936689 0.091068 0.008293
Approximation of Diffusion 50 0.989168 0.040020 0.001601
60 0.992544 0.035883 0.001287
70 0.862132 0.148683 0.022106
80 0.948769 0.141889 0.020132
Logistic 50 0.977668 0.051396 0.002641
60 0.944571 0.084730 0.007179
70 0.880337 0.119961 0.014390
80 0.895319 0.143419 0.020569
Midilli 50 0.988562 0.041124 0.001691
60 0.994386 0.031134 0.000969
70 0.988197 0.043502 0.001892
80 0.999999 0.000520 0.0000002
Aghabashlo model 50 0.988777 0.033260 0.001106
60 0.995480 0.021639 0.000468
70 0.988449 0.033335 0.001111
80 0.999796 0.005156 0.000002

from 4.10±0.96 to 5.38±0.06 at different drying methods. In pulp increased, the lightness, redness, and yellowness values
general, as the drying temperature increased, the lightness decreased. The researchers attributed this change in color to
value increased and the redness decreased. Sahu et al. [50] the fact that when the drying temperature is increased, the
found that as the drying temperature of foam-dried jamun reducing sugars bind with an amino group protein, causing

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Table 3  Physical properties of Sample L* a* b* pH Water activity Dry matter (%)

foam-dried cornelian cherry
pulp powder LS 63.59 ±1.02 b
28.29 ±4.04 a
4.10 ±0.96a
4.56 ±0.02 a
0.2094 ±0.0009 c
92.08 ±2.07b
CD50 63.15 ±0.06b 31.57 ±0.61a 5.38 ±0.06a 4.36 ±0.10b 0.3272 ±0.0081a 93.79 ±0.49ab
CD60 64.21 ±0.63ab 30.45 ±0.24a 5.21 ±0.07a 4.42 ±0.11b 0.2456 ±0.0077b 95.29 ±0.21a
CD70 66.35 ±1.32a 27.46 ±1.98a 4.66 ±0.49a 4.44 ±0.02ab 0.2494 ±0.0076b 95.92 ±0.35a
CD80 65.14 ±0.15ab 29.23 ±0.39a 5.21 ±0.03a 4.42- ±0.08b 0.2112 ±0.0023c 96.36 ±0.02a

L*, a*, and b* are color parameters. FDS Freeze-dried sample; CD50 convective dried sample at 50°C;
CD60 convective dried sample at 60°C; CD70 convective dried sample at 70°C; CD80 convective dried
sample at 80°C
*There is no statistical difference between the means marked with the same letter (p > 0.05)

methods. They observed that the use of egg white powder

accelerated the browning reaction, the L* value increased,
and the a* and b* values decreased compared to freeze-
drying and hot air. These results were inconsistent with our
study. In the present study, the b* (yellowness) value of the
powders obtained by the freeze-drying method is lower than
the convective-dried ones. There was no statistically signifi-
cant difference between a* values (p>0.05).
Depending on the drying method applied, the samples
obtained were characterized by water activity ranging from
0.2094 to 0.3272, which is shown in Table 3. The lowest
Fig. 2  Images of foamed cornelian cherry powder samples dried by water activity was determined in the freeze dried powder. It
convective drying at 50, 60, 70, and 80°C (from left to right) can be assumed that the obtained products were microbio-
logically stable.
the Maillard reaction and the breakdown of the total antho-
cyanin content. 3.4 Flowability, cohesiveness, and solubility
It has been determined in various studies that foaming
agents and foam stabilizers affect color parameters. Gao The fluidity and stickiness of the powders were evaluated as
et al. [12] reported that egg white powders added to the foam the Carr index (CI) and Hausner ratio (HR). The flowability
had a diluting effect on the color in their study on blueberry. is used to determine the free flow properties of the powder.
They observed that L*, a*, and b* values tended to decrease A suitable powder flow is important for both consumers and
by increasing the carboxymethyl cellulose stabilizer from 0 manufacturers [53]. The density, flow properties and solubil-
to 1%. Ng and Sulaiman [51] investigated the physicochemi- ity of powders are given in Table 4.
cal properties of powders produced from red beet using egg According to the CI, it was observed that the fluidity
albumin, maltodextrin, and fish gelatin. They reported that was between 18 and 22% and increased as the temperature
control samples of beets without maltodextrin showed lower increased (Table 4). Results between 15 and 20% were rated
L*, a*, and b* values than those containing 10% egg albu- as “good” as classified by Hajiaghaei and Sharif [53]. The
min. They reported that the increase in L* value was due to stickiness of the powders, HR, results were between 0.77 and
the white color of maltodextrin. In a study on tomatoes, it 0.81. In Hajiaghaei and Sharif [53], samples with (<1.2) val-
was observed that a* values increased with increasing dry- ues according to their classification were evaluated as “low”
ing temperature, egg albumin, and carboxymethyl cellulose adhesiveness. Sahu et al. [50] observed that fluidity values
concentration. It is thought that non-enzymatic reactions are increased as the drying temperature increased for foam-dried
effective in the structural degradation of various pigment jamun pulp, in agreement with our findings. They stated that
compounds [52]. Hajiaghaei and Sharif [53] carried out the increased value in flowability with higher temperature
foam drying in red beet and quince fruit with 0–10% malto- of drying may be due to the reduction in moisture content.
dextrin. They observed that the color results of the powders A higher HR means the powder is more sticky and less
obtained by hot air and freeze-drying methods were different free-flowing. The cohesiveness of dust particles is mostly
from each other, and the L*, a*, and b* values of the freeze- affected by interparticle forces as well as other factors such
dried ones were lower, which is consistent with our data. as mechanical interlocking [53]. Furthermore, the solubil-
Çalışkan Koç et al. [54] foam dried taro fruit using different ity of powders is an important factor in the production of

13
Biomass Conversion and Biorefinery

Table 4  Flow properties of Sample Bulk density (g/cm3) Tap density (g/cm3) CI HR Solubility (%)
foam-dried cornelian cherry
pulp powder LS 0.35 ±0.01 d
0.43 ±0.01c
18.61 ±0.43 a
0.81 ±0.01a
83.70 ±0.97a
CD50 0.44 ±0.01c 0.55 ±0.00b 19.83 ±2.10a 0.80 ±0.02a 82.26 ±0.50a
CD60 0.54 ±0.04a 0.68 ±0.06a 20.56 ±1.39a 0.79 ±0.01a 82.46 ±0.34a
CD70 0.53 ±0.01ab 0.67 ±0.01a 21.66 ±2.70a 0.77 ±0.02a 82.94 ±0.18a
CD80 0.48 ±0.01bc 0.62 ±0.01ab 22.77 ±2.31a 0.79 ±0.02a 80.00 ±0.96b

CI Carr index, HR Hausner ratio, LS freeze-dried sample, CD50 convective dried sample at 50°C, CD60
convective dried sample at 60°C, CD70 convective dried sample at 70°C, CD80 convective dried sample at
80°C
*There is no statistical difference between the means marked with the same letter (p > 0.05)

fruit powders. Fruit powders with poor solubility provoke obtained by lyophilization appear more uniform than those
challenges during processing resulting in economic losses. obtained by the convective method may indicate a possi-
For food powders to be useful and functional, they must ble more homogeneous water removal process. It has been
have high solubility in the aqueous phase [55]. The solubility observed that the structure at 60 and 70°C is rougher and
values of the convective dried ones were close to the lyophi- more complex than at 50°C and 80°C. The rough and com-
lized powders. The lowest solubility value was obtained in plex structures at 60 and 70°C may indicate that drying
those dried at high temperatures. processes in certain temperature ranges affect the intrinsic
properties of the material. It has been observed that the most
3.5 Scanning electron microscopy suitable samples according to the morphological structure
are the samples dried at 50 and 80°C, and by lyophilization.
SEM was used to examine the morphological structure of The fact that the most suitable samples according to mor-
dried CC powders. It is observed that the appearance of the phological structure are those lyophilized and dried at 50 and
powders obtained by lyophilization is smoother than those 80°C may suggest that these temperatures provide optimal
obtained convectively (Fig. 3). The fact that the powders water removal conditions for the material. Seerangurayar

(a) (b) (c)

(d) (e)

Fig 3  Microstructural images of foamed cornelian cherry powder samples dried under different conditions: a convective dried sample at 50°C; b
convective dried sample at 60°C; c convective dried sample at 70°C; d convective dried sample at 80°C; and e lyophilized sample

13
 Biomass Conversion and Biorefinery

et al. [14] found that in the particle morphology of palm for carboxyl and ester groups can be found between 1640
powders obtained by foam drying using maltodextrin and and 1720 ­cm−1 [58]. The presence of amide Ι (stretch vibra-
gum Arabic, using an agent is necessary to obtain a fluid tions of C=O and C-N groups) and amid II (mainly from
powder and the particles appear smoother and larger depend- N-H bending) at absorbing wavelengths between 1700–1500
ing on the sugar content. The wrinkling on the surface is ­cm−1 and 1500–1300 c­ m−1 proves the presence of the pro-
directly proportional to the concentration ratios of the agents tein. The variation in the band region between 1400 and
used [56]. 1100 ­cm−1 is due to the OCH, CCH, and COH bending
vibrational modes of carbohydrates [59, 60]. Peaks related
3.6 FTIR spectra of powder samples to phenolic compounds were found in regions between 1600
and 900 ­cm−1. For example, the bond around 1640 c­ m−1 pre-
FTIR spectra of cranberry fruit are shown in Fig 4. Three dominantly belongs to the C-C bond vibrations of phenolic
characteristic regions are observed in the spectrum between compounds [61]. In the third region, C-O-H bonds and C-O,
3600 and 2500, 2000 and 1300, and 1350 and 700 c­ m−1. C-O-C glycosidic bonds are found in the region between
The bands in the 3400–3000 c­ m−1 region are typically con- 1150 and 700 ­cm−1 [62]. The last spectral region, that is,
nected to various hydroxyl (OH) stretching vibrations. The the part below 900 ­cm−1, is the fingerprint responsible for
OH stretching vibrations witnessed can be greatly influenced the crystal field showing the conformational changes in the
by hydrogen bonding, so they depend on the strength of the material.
hydrogen bonds. The range of 3000–2900 ­cm−1 was assigned
to the symmetrical and asymmetric stretching vibration 3.7 Polyphenol content
of the C-H band and the stretching vibration of the N-H
band, corresponding to both the alkyl and aromatic groups, CC fruit contains a significant amount of antioxidant antho-
respectively [57]. In the second region, absorption bands cyanins and phenolic compounds [39]. Total phenolics,

Fig. 4  FTIR spectra of cornelian cherry powders: a FTIR spectra of convective dried fruit at different temperatures, and b FTIR spectra of lyo-
philized fruits and lyophilized foam

13
Biomass Conversion and Biorefinery

total flavonoids, and total anthocyanins of CC pulp used the TACN decreased. The TACN of samples dried at 50°C
in this study were determined as 32.81±0.22 mg GAE/g, is significantly lower than at other temperatures. However,
12.83±0.56 mg ECE/g, and 4.69±1.23 mg CGE/g in dry samples dried at 60°C and 70°C gave better results in terms
matter, respectively. In the literature, total phenolics for CC of TACN than at other temperatures. This shows that certain
fruit have been reported as 2.61–26.96 mg/g [63–66], total temperature conditions have a complex effect on the deg-
flavonoids as 0.54–6.69 mg/g [65, 67], and total anthocya- radation processes of anthocyanins and that sometimes an
nins as 1.07–8.50 mg/g [63, 65, 68]. Table 5 shows the TPO, increase in temperature can increase color stability, contrary
TF, and TACN, and antioxidant activity of foam-dried CC. to expectations. This may be due to the fact that anthocya-
The TPO of CC powders was found to range from 15.97 nins have a dynamic chemical structure that can enter into
to 16.33 mg GAE/g powder. The TPO value of the lyophi- complex reactions and turn into different products depend-
lized sample has a higher value than the convective dried ing on temperature. Tepić Horecki et al. [73] compared the
ones. Of the convective dried ones, the samples dried at TACN of CC for different drying methods. They calculated
50°C and 60°C had a lower TPO value than the other tem- the TACN in fresh fruits as 14.70 mg/g. They determined
peratures. High temperatures can reduce TPO values by the highest anthocyanin content in samples dried under
accelerating oxidative degradation. The TF of CC powders vacuum at low temperature (40°C), significant anthocya-
is shown in Table 5 ranging from 0.94 to 1.29 mg QE/g nin loss was detected in samples dried at high temperatures
powder. Total flavonoid values were lowest in lyophilized (60–80°C) and in the sun. Zia and Alibas [4] dried CC fruits
samples, while the highest was measured in samples dried at 50, 70, and 90°C and found their TACN to be 1.05, 2.62,
at 80°C. Danielewski et al. [69] reported that the TPO in CC and 0.63 mg/g, respectively. Our results agree with these
extract was 25.46 mg GAE/g and TF was 18.51 mg QE/g. results, high temperature caused anthocyanin loss. Kitchen
Gupta et al. [70] showed that foam mat drying protects phe- et al. [74] investigated the effects of drying temperature on
nolic compounds in jujube juice and increases antioxidant anthocyanins of vacuum belt dried blueberry pulp powder
activity. In addition, increased foaming agent concentration and found that anthocyanins decreased with increasing dry-
helped preserve phenolic compounds. Brar et al. [71] investi- ing temperature. Darniadi et al. [75] examined the individual
gated the effect of process parameters on the drying of peach anthocyanin profiles of blueberry powders obtained by foam
fruit by foam mat drying method. They determined that the mat freeze-drying and spray-drying methods and observed
most suitable process parameters to obtain the highest TPC higher levels of anthocyanin compounds in blueberry pow-
of dried peach powder were 12% peach concentration, 900 der obtained by foam mat freeze-drying method. Reis et al.
rpm whipping speed, 50°C drying temperature, and 360 min [76] stated that foam mat drying can increase the stability of
drying time. Jakkranuhwat and Kunchansombat [72] found anthocyanins in plant foods, maintain the integrity of antho-
that the processing of purple-fleshed sweet potato powder cyanins and increase the anthocyanin content. Darniadi et al.
with foam drying resulted in a decrease in TPC and TACN [77] investigated the effects of different matrix materials and
with an increase in temperature and volume change param- stabilizers (trehalose, β-lactoglobulin, and bovine serum
eters during the foam drying process. albumin) for foam drying processes based on blueberry
Anthocyanins play an important role in determining the juice. They showed that the matrix materials and stabilizers
antioxidant capacity of the samples. They are bioactive used during foam drying processes can have a significant
substances that degrade at high temperatures. The lyophi- effect on the stability and composition of anthocyanins.
lized sample had the highest TACN at 0.53 mg/g, while the It is important to highlight that further studies are needed
lowest anthocyanin content was found in samples dried at to characterize the polyphenol profile of the products formed
80°C with 0.32 mg/g. As the drying temperature increased, and assess the effect of drying temperature on specific

Table 5  (Poly)phenol content Sample TPO (mg GAE/g) TF (mg QE/g) TACN (mg CGE/g) FRAP (mmol/g) DPPH (mmol/g)
and antioxidant activity of
foam-dried cornelian cherry LS 16.33 ±0.07 a
0.94 ±0.20 a
0.53 ±0.03 a
58.84 ±0.50 ab
46.10 ±5.34ab
pulp powder
CD50 15.97 ±0.02b 1.02 ±0.02a 0.36 ±0.02c 55.52 ±3.48b 39.77 ±2.95b
CD60 15.94 ±0.12b 1.17 ±0.15a 0.48 ±0.01ab 57.20 ±3.00ab 52.65 ±4.01a
CD70 16.14 ±0.03ab 1.11 ±0.21a 0.40 ±0.04bc 60.56 ±1.32ab 44.62 ±2.80ab
CD80 16.14 ±0.11ab 1.29 ±0.03a 0.32 ±0.04c 62.85 ±2.64a 52.42 ±2.57a

TPO Total phenolic content; TF total flavonoid content; TACN total anthocyanin content; FRAP ferric ion
reducing antioxidant power; DPPH 2,2-diphenyl-1-picrylhydrazyl, LS lyophilized sample; CD50 convec-
tive dried sample at 50 C; CD60 convective dried sample at 60°C; CD70 convective dried sample at 70°C;
CD80 convective dried sample at 80°C
*There is no statistical difference between the means marked with the same letter (p > 0.05)

13
 Biomass Conversion and Biorefinery

phenolic acids, flavanoids, and anthocyanins that are known the best preservation of antioxidant compounds in CC pulps.
for their remarkable bioactive properties. FRAP values increased when the phenolics were high. In
other words, FRAP values were better preserved due to the
3.8 Antioxidant activity better preservation of phenolic compounds. In addition,
higher FRAP values at 70–80°C may be an indication that a
Antioxidant activities of dried samples were performed mild Maillard reaction occurs when these temperatures are
with two different methods, and the results are presented increased, and as a result, new antioxidant compounds are
in Table 5. DPPH and FRAP values of CC pulp used in formed. The Maillard reaction is a complex reaction that
this study were determined as 311.60±16.70 mmol/g, and occurs as a result of the reaction between proteins and carbo-
228.10±20.40 mmol/g in dry matter, respectively. FRAP and hydrates, and the compounds formed as a result of this reac-
DPPH values of cornelian cherries were previously reported tion are known to have antioxidant properties. Zielinska and
as being between 41 and 149 μmol/g dw [63, 78], and 33.41 Zielinska [83] determined the antioxidant activities of dried
and 39.89 μmol Trolox/g in fresh weight [79], respectively. CC with different drying methods. They determined that the
As can be seen, the DPPH and FRAP values of the sam- antioxidant activities of the samples dried by the microwave-
ples varied significantly depending on the drying method vacuum drying method were better preserved than those
and temperature (p>0.05). High-temperature convective dried by the conventional drying method. Oszmiański et al.
drying had a higher DPPH free radical scavenging effect. [84] convective and freeze-dried CC and found that convec-
Lyophilization minimizes oxidative degradation of phenolic tive-dried ones showed higher FRAP values. Michalska et al.
compounds, especially anthocyanins, by allowing water to [85] investigated the effect of different drying conditions
directly transition into a solid state under low temperature (temperature, airflow) on the antioxidant properties of black
and vacuum; this contributes to the maintenance of high currant pulp, which was ground into powder, and found that
antioxidant activity and long shelf life of the samples. The the powders dried at low temperature (50°C) had high anti-
significant protection of the phenolic compound, especially oxidant capacity.
anthocyanin content, of the lyophilized samples, led to high Although the methods used to assess the antioxidant
antioxidant activity. Drying at 60 and 80°C had the highest power of the developed samples are valid, accurate, and
DPPH free radical removal effect. However, the differences quantitative; yet they have some limitations. These meth-
in other temperature levels are not statistically significant. ods may not represent the biological system in which the
The lowest DPPH free radical scavenging effect was found polyphenols would act as antioxidants. The complexity and
in the powders produced by the convective drying process biological interactions that happen in the human body are
at 50°C. Cosmulescu et al. [67] found that the DPPH free not considered in these assays. In addition, different polyp-
radical scavenging effect in various genotypes of cranberry ehnols or other antioxidants may have different mechanisms
ranged from 1.24 to 2.71 mmol Trolox/100 g. According of action—such as regulating cellular antioxidant pathways
to this study, it has been shown that there is a significant which are not considered in these assays.
difference in the antioxidant capacity of CC under different
conditions and the use of different methods also affects the 3.9 Bioaccessibility of product
results of the analysis. Petkova and Ognyanov [80] stated
that the lowest antioxidant activity was in dried CC (46–48 The highest bioaccessibility of total phenolic compounds
mM TE/g), therefore, storing CC as a compote has a prom- was obtained in the samples prepared by the lyophilization
ising antioxidant potential. Wojdyło et al. [81] stated that process (Table 6). In the drying processes at other tempera-
drying fruit at high temperatures can reduce the antioxidant ture levels, the bioaccessibility of total phenolics was lower.
activity, and they found that cherries dried at 70°C had lower This result shows that the lyophilization process prevents the
antioxidant capacity than those dried at lower temperatures. loss of phenolic compounds in CC and the bioactive compo-
Zia and Alibas [4] found a decrease in the antioxidant activi- nents of the fruit are better preserved. However, based only
ties of DPPH, ABTS, and FRAP as the drying temperature on the total phenolic content, it is not possible to say that CC
increased. They noted that the samples dried at 50°C had foam drying provides less bioactive component protection
higher antioxidant activity. Tepić Horecki et al. [73] stated compared to drying processes at other temperature levels.
that as the drying temperature increases, the antioxidant The bioaccessibility of flavonoids and anthocyanins was not
activity decreases. Skrovankova et al. [82] found that the investigated in the current study which is considered one
antioxidant activity in CC could increase with drying time, of the limitations. A previous study [86] investigated the
and the increase measured after drying was approximately effect of foam drying on red sorghum at different tempera-
1.3 times higher than before drying. tures (60–80°C) on bioaccessibility. The results showed that
FRAP data show that lyophilization and drying at 80°C foam drying at high temperatures reduced the bioaccessibil-
resulted in high antioxidant activity. Lyophilization provided ity of proanthocyanidins in sorghum extract. This is because

13
Biomass Conversion and Biorefinery

Table 6  Bioaccessibility of Sample Bioaccessibility (%) terms of both physical and antioxidant properties. The high-
total phenolic compounds of est bioaccessibility value was determined in the lyophilized
foam-dried cornelian cherry LS 21.66 ±2.84a
pulp powder
samples, and there was no statistical difference depending
CD50 14.48 ±1.07b on the drying temperatures in the convective dried samples
CD60 14.37 ±0.69b (p>0.05). When evaluated in terms of the temperatures used
CD70 13.08 ±0.10b in drying, it can be said that a different temperature is bet-
CD80 13.05 ±0.06b ter for each of the investigated parameters. Considering the
LS Lyophilized sample; CD50 convenience and cost, it was concluded that CC pulp can be
convective dried sample at used in convective dryers for foam drying. This powder can
50°C; CD60 convective dried be used in many food products, such as beverages, sweets,
sample at 60°C; CD70 con- and can be a convenient agent for synthetic additives.
vective dried sample at 70°C;
CD80 convective dried sample Availability of data and materials Data available within the article or
at 80°C its supplementary materials
*There is no statistical differ-
ence between the means marked Author contribution Beyza Kaba: methodology, investigation, for-
with the same letter (p > 0.05) mal analysis, writing—original draft. Yasemin Yıkılkan: methodol-
ogy, investigation, formal analysis, writing—original draft. Hojjat
Pashazadeh: formal analysis, data curation, writing—original draft.
oxidative damage at high temperatures reduces antioxidant Ali Ali Redha: validation, writing—original draft, writing—review
capacity. However, no reduction in bioaccessibility of proan- and editing. Ilkay Koca: conceptualization, supervision—project
thocyanidins was observed when foam drying at low tem- administration.
peratures was applied. It has been reported that foam drying
had higher bioaccessibility than other drying methods [75]. Declarations
It is important to highlight that the determination of the Ethical approval and consent to participate Not applicable.
bioaccessibility of compounds by in vitro digestion has
limitations and may not reflect the true gastrointestinal con- Consent for publication Not applicable.
ditions. The bioaccessibility of polyphenols is affected by
Competing interests The authors declare no competing interests.
the gut microbiota, and those microorganisms contribute
to the breakdown of large polyphenols into smaller com-
Open Access This article is licensed under a Creative Commons Attri-
pounds that are more bioaccessible and can pass through bution 4.0 International License, which permits use, sharing, adapta-
the intestinal wall into the blood stream. The experimental tion, distribution and reproduction in any medium or format, as long
method used did not consider the gut microbiota. In addi- as you give appropriate credit to the original author(s) and the source,
provide a link to the Creative Commons licence, and indicate if changes
tion, the product formed can potentially be a functional food
were made. The images or other third party material in this article are
ingredient, thus it would be incorporated into a product. The included in the article’s Creative Commons licence, unless indicated
new matrix (product formed) will be different in comparison otherwise in a credit line to the material. If material is not included in
to the raw material (CC powder), and this can influence the the article’s Creative Commons licence and your intended use is not
permitted by statutory regulation or exceeds the permitted use, you will
bioaccessibility of polyphenols. Thus, further experiments
need to obtain permission directly from the copyright holder. To view a
are required to assess the bioaccessibility of the formulated copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.
powder.

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