LWT - Food Science and Technology 154 (2022) 112841

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LWT
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The effects of selected stabilizers addition on physical properties and

changes in crystal structure of whey ice cream
Anna Kamińska-Dwórznicka a, *, Sylwia Łaba b, Ewa Jakubczyk a
a
Department of Food Engineering and Process Management, Institute of Food Sciences, Warsaw University of Life Sciences (WULS-SGGW), Nowoursynowska 159C, 02-
776, Warsaw, Poland
b
Institute of Environmental Protection-National Research Institute, Krucza 5/11d St., 00-548, Warsaw, Poland

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

Keywords: Dry sweet whey was used in this study at 42% to prepare a new ice cream composition. The additional aim of the
Recrystallization research was to select the most effective stabilizers in ice recrystallization inhibition. The addition and impact of
Stabilizing mixes two stabilizing systems, containing LBG (locust bean gum), guar gum and respectively κ- and ι-carrageenan, on
Whey ice cream
physicochemical properties (density, pH, overrun, viscosity, melting time) and crystal structure of ice cream after
a specified storage time of: 24 h, 1 month and 3 months were examined. It was found that whey presence in­
creases the density and viscosity and reduces the overrun of the analyzed product. Addition of stabilizing mixes
also differentiated density (higher for the samples with additives), melting time and overrun. The lowest overrun
value and simultaneously the shortest melting time were recorded for ι-carrageenan addition. No influence of
stabilizing systems on pH of examined ice cream was found. The stabilizing mix containing ι-carrageenan was
found to be the best in recrystallization inhibition, demonstrated by the presence of crystals with the smallest
diameter 28 μm, after 3 months of storage, while for the sample without additives 68 μm was noted.

1. Introduction
Sweet whey is a co-product from dairy manufacture, generated
during the production of rennet-type cheese. This co-product is recog­
nized as highly nutritional and biologically valuable. It contains mainly
water, proteins that are rich in sulfurated and essential branched chain
amino acids, lactose, vitamins, minerals and fats. Whey proteins repre­
sent at least 20% of the protein constituting bovine milk: 70% are
β-lactoglobulin (β-lg), α-lactoalbumin (α-la) and glycol-macro-peptide.
Subfractions such as lactoferrin, lysozyme and lacto-peroxidase are
present in a smaller concentrations (Faucher, Perreault, Gaaloul, &
Bazinet, 2020; Maciel et al., 2020). The lipids found in sweet whey
represent two-thirds of the total lipid content and consist of tri­
glycerides, the rest being polar lipids, mostly phospholipids (Faucher
et al., 2020). The dairy industry is still struggling to find application for
different types of whey. A potential new nutritional product is
whey-based manufactured ice cream. Dry sweet whey has already been
used successfully in ice cream at low concentrations, but the use of large
quantities promoted the development of sandiness probably as a
consequence of lactose crystallization (Parsons, Dybing, Coder,
Spurgeon, & Seas, 1985; Thompson, Reniers, Baker, & Siu, 1983).
Ice cream is a frozen dessert made by freezing a mix of milk, yoghurt
or fruits, sugar, stabilizer, and emulsifier, with or without eggs (Adapa,
Schmidt, Jeon, Herald, & Flores, 2000; Clarke, Buckley, & Lindner,
2004). Typical ice cream is approximately 30% ice, 50% air, 5% fat, and
15% is a continuous phase, the so-called matrix (sugar solution – su­
crose, glucose and lactose), (Wildmoser, Scheiwiller, & Windhab, 2004).
The formation of ice crystals determines final quality of ice cream. Ice
crystal sizes between 10 and 20 μm are important attributes to give the
product its desired texture. Larger ice crystals, if present in sufficient
number, confer a grainy texture to the final product (Haddad Amamou,
Benkhelifa, Alvarez, & Flick, 2010; Arellano et al., 2011; Kamińska-D­
worznicka, Gondek, Laba, Jakubczyk, & Samborska, 2019; Kamin­
ska-Dworznicka, Janczewska-Dupczyk, Kot, Laba, & Samborska, 2020).
Ice formation accelerates in the first hours after ice cream produc­
tion. Under unstable temperature conditions or during long-term stor­
age, especially below the glass transition temperature, an unfavorable
recrystallization process may occur (Hagiwara & Hartel, 1996).
Recrystallization is the melting of some small crystals, and the growth of
the existing ones due to two mechanisms: coalescence and migration.

* Corresponding author.
E-mail address: anna_kaminska1@sggw.edu.pl (A. Kamińska-Dwórznicka).
URL: http://www.wnoz.sggw.pl (A. Kamińska-Dwórznicka).

https://doi.org/10.1016/j.lwt.2021.112841
Received 5 August 2021; Received in revised form 18 November 2021; Accepted 19 November 2021
Available online 30 November 2021
0023-6438/© 2021 The Authors. 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/).
A. Kamińska-Dwórznicka et al.
Coalescence is the process of two or more adjacent ice crystals joining
into one. Migration (Ostwald maturation) consists of two stages: melting
of smaller crystals and the movement of free water to the surface of
larger crystals. The driving force of this migration is the difference in
partial pressures that occurs on these surfaces. Typically, these two
recrystallization mechanisms occur simultaneously (Kaminska-Dworz­
nicka et al., 2019; Kamińska-Dwórznicka, Skrzypczak, & Gondek, 2016;
Regand & Goff, 2003).
In order to modify water-binding capacity, freezing rates, rheological
properties and ice crystal growth, stabilizers are commonly used (Adapa
et al., 2000; Kaminska-Dworznicka et al., 2019; Kamińska-Dwórznicka,
Antczak, Samborska, & Lenart, 2015; Kamińska-Dwórznicka, Matusiak,
et al., 2015). Different fractions of carrageenan’s (usually a commercial
mix) are commonly used dairy stabilizers. Kappa- and iota-carrageenan
in comparison to the rest of the carrageenan fractions are most often
used in the production of ice cream and other desserts. Kappa and iota
contain, respectively, one and two sulfate groups per disaccharide,
which give them different properties (Necas & Bartosikova, 2013).
Kappa carrageenan reacts with potassium ions, forming a brittle and
hard gel. The iota fraction creates a soft-elastic gel, which is the result of
interaction with calcium ions (Bui, Nguyen, Nicolai, & Renou, 2019;
Kaminska-Dworznicka et al., 2020; Necas & Bartosikova, 2013). Kappa
gels shows stability during freezing and thawing and shows a more
visible stabilizing effect mixed with starch. Iota carrageenan works more
effectively in combination with LBG (locust bean gum) and this com­
bination is more prone to syneresis (Blakemore & Harpell, 2010).
The objective of the present investigation was therefore to evaluate
the impact of both ι- and κ-carrageenan on physical properties and
crystal structure of whey ice cream frozen and stored 1 day, 1 month and
3 months. While in traditional ice cream the iota fraction usually worked
better for stabilization this comparison of two carrageenan fractions
allowed for the selection of a better stabilizer for whey ice cream.
2. Materials and methods
2.1. Preparation of whey ice cream
For each experimental variant 1 L of ice cream mix was prepared
from: 42.00% sweet whey powder (Mlekovita, Poland), 8% sucrose milk
powder lactose free (Mlekovita, Poland), 0.40% Amaretto syrup (Monin,
France), from 49.05 to 49.20% water, 0.40% emulsifier E471 (FOODING
Shanghai) and 0.23% of stabilization mix - three different variants:
re: (reference sample) without any stabilizers,
K mix: 0.1% LBG + 0.1% GG + 0.03% κ-carrageenan (Fluka, Sigma-
Aldrich),
I mix: 0.1% LBG + 0.1% GG + 0.03% ɩ-carrageenan (Fluka, Sigma-
Aldrich).
• LBG – locust bean gum and GG – guar gum (FOODING Shanghai)
After mixing all ingredients and stabilizers, part of the whey ice
cream mix was tested for the physical properties analysis and part was
then frozen in a small freezer Gelato PRO 1700 (Nemox, Italy), for 40
min, freezing temperature − 20 ◦ C. Then the samples were packed into
plastic boxes (at least 2 boxes for 300 ml for each variant), transported
and stored for further microscopy analysis, for 24 h, 1 month and 3
months at − 18 ◦ C.
2.2. Determination of physicochemical properties
2.2.1. Density
Density of the ice cream mix was determined by the pycnometric
method, described by Dłużewska, Gazda, & Leszczyński, 2003. A glass
pycnometer was filled to 25 cm3 and for every sample the weight of this
volume was taken at the temperature of 20 ◦ C. The test was performed in
duplicate.
2
LWT 154 (2022) 112841
2.2.2. Ice cream overrun
The overrun of ice cream was determined according to the following
formula (Dłużewska et al., 2003; Góral et al., 2018):
w1 − w2
O [%] =
w2
⋅100%
where: w1 mass of unit volume of mixture (g), w2 mass of unit volume of
ice cream (g).
2.2.3. Viscosity
The viscosity of the ice cream mix was determined using a Haake
MARS 40 rheometer (Thermo Scientific, Japan). The measurements
were carried out with a CCB/CC25 DIN/Ti concentric cylinder geometry
(gap size 5.3 mm) within the shear rate of 0–100 s− 1 at a constant
temperature of 25 ◦ C. All measurements were done in triplicate for each
kind of ice cream mix. The data obtained from RheoWin v.4.86. Job
Manager (Thermo Scientific, Karlsruhe, Germany) were plotted with
apparent viscosity (ηapp) as a function of shear rate (γ̇) in the semi-
logarithmic scale (the viscosity curves). The flow behavior was also
analyzed and obtained data were fitted to the following model:
Herschel-Bulkley:
ηapp = τ0 (γ̇)− 1 + K γ̇n− 1
(1)
where: ηapp – the apparent viscosity (Pa s), γ̇ –the shear rate (s− 1), ηp –the
plastic viscosity (Pa s), τ0– yield stress (Pa), K – the consistency index (Pa
sn), n – flow behavior index (dimensionless).
The adequacy of fitted models was estimated using the regression
analysis which delivered the correlation coefficient (R).
2.2.4. pH
pH value was measured with the Electrode Elmetron EPP3t with the
temperature sensor Pt–1000B, by dipping in liquid at 25 ◦ C. The test was
performed in duplicate.
2.2.5. Melting time
To determine the melting time, a cooled metal ring (stored at − 25 ◦ C
for 24 h; 35 mm in height and 25 mm in diameter, volume 25 ml) was
filled with ice cream after preparation and then stored for 24 h at
− 25 ◦ C. After storage the ring was placed on the funnel with two pins
located at the ends of the ring at the controlled temperature of 25 ◦ C. The
time required for dripping of the first drop of melted ice cream was
recorded (Dłużewska et al., 2003; Góral et al., 2018).
2.3. Microscopy and image analysis
To prepare the samples for image analysis (after: 24 h from the
production cycle, 1 month and a 3 months), a small piece of ice cream
was taken from the center of the plastic box or cylindrical vessel, from at
least 3 different locations, a minimum of 3 cm away from the ice cream
surface, and placed on an object slide using a spatula and then covered
with a cover slip placed on the top of the sample. Pressing the sample
reduced the overlap of ice crystals to discern them individually and
destroy the air cell structure to provide excellent clarity. Samples were
prepared in a freezing chamber and transferred to a microscope with the
cooling system Linkam Scientific PE 94.
The recrystallization process was analyzed based on the images of ice
crystals taken after preparation. A microscope (Nikon Alpha Phot-2)
with the cooling system Linkam Scientific PE 94 and a camera (Nikon
DS-Fi1) were used. The obtained images were then analyzed using NIS
Elements D software. From 300 to 500 crystals were marked for
particular sample, and then area, equivalent diameter and standard
deviation were calculated using the NIS Elements D Imaging software
(ver. 3.00, Nikon).
A. Kamińska-Dwórznicka et al.
2.4. Statistical analysis
In order to determine the effect of the stabilizer addition, the one-
way ANOVA test was used. Further tests to assess the significance of
differences between particular groups were performed: Student’s T-test
was applied to compare independent samples in pairs, and variance
analysis (ANOVA) was used for more than two groups. Detailed analysis
was based on Tukey’s confidence intervals. All statistical tests were
carried out at significance level of α = 0.05. Statistical processing of
results was performed using the program Statistica 13.1.
The frequency distribution of crystals size was computed using
Microsoft Excel 2011 macro data analysis. The relative frequency of any
class interval was calculated as the number of the crystals in that class
(class frequency) divided by the total number of crystals, and expressed
as a percentage (Figs. 2 and 3). According to the method described by
Regand & Goff, 2003, the parameter X50 was analyzed, as the mean
diameter (DA) for 50% of crystals in the sample. The mean diameter (DA)
and standard deviations (SD) of each class were also calculated
(Table 3). The method has been described previously (Goff & Hartel,
2013; Kamińska-Dwórznicka, Matusiak, et al., 2015; Kamińska-Dwórz­
nicka et al., 2016; Kot Anna, 2020).
3. Results and discussion
3.1. Physicochemical characteristics of whey ice cream
The ice cream mix density significantly affects appropriate consis­
tency and the smoothness of the final product. The increase of ice cream
mix density is not a desirable factor, because it could affect inappro­
priate product overrun (Florowska, Wójcik, Florowski, & Dluzewska,
2013). Consequently mixture overrun has a great influence on ice cream
texture. Too high density of the ice cream mix may increase ice cream
hardness and deteriorate its sensory qualities. Goff and Hartel (2013)
reported the density of milky ice cream in the range from 1.0544 to
1.1232 g/cm3. In this research the density of ice cream mixes was in the
range from 2.18 g/cm3 for the sample without any additives (re)
2.60–2.62 g/cm3 for ice cream with LBG, guar gum and respectively
kappa (K mix) and iota carrageenan (I mix) (Table 1). Based on the
results of the ANOVA test, stabilizer addition significantly altered ice
cream mix density when compared to the sample without additives
(p-value < 0.05) and it was higher than the usual density measured for
classic milky ice cream (around 1 g/cm3). According to (Dłużewska,
Grodzka, & Mosiewska, 2005) this effect could be related to the high
Fig. 1. Ice crystal size distribution in whey ice cream without stabilizers after different times of storage at − 18 ◦ C.
3
LWT 154 (2022) 112841
whey protein content, since when they increased whey protein amount
from 3.12 to 6.25% in milky ice cream the density also rose from 0.85 to
0.92 g/cm3. The increasing density of ice cream contributes to reduction
of its aeration, which increases its hardness (Dłużewska et al., 2005;
Jasińska, Trzciński, Dmytrów, & Mituniewicz-Małek, 2012).
The ice cream overrun ranged from 11.93 to 15.82% (Table 1). The
type of stabilizer significantly differentiated the ice cream overrun (p-
value < 0.05). It was found that the overrun was higher for the ice cream
with LBG, guar gum and kappa carrageenan addition (K mix). For the
ice cream without additives (re) it was at the level of 12.91%, whereas
for traditional milky ice cream without additives overrun was around
50% (Elsabie & Aboel Einen, 2017). Surprisingly, the lowest overrun
was noted for the sample with iota carrageenan addition (I mix)
(Table 1). Usually for milky ice cream iota carrageenan addition caused
an increase in the overrun value, which was related to the interaction
with the protein molecule (Soukoulis, Chandrinos, & Tzia, 2008). This
result could suggest that whey protein influences aeration to a lower
extant than other types of milk protein. On the other hand, reducing ice
cream fat content caused a decrease in overrun (Tiwari, Sharma, Kumar,
& Kaur, 2015). Additionally, Dłużewska et al. (2003) observed that the
ice cream overrun was inversely proportional to the LBG content in the
mixtures. Góral et al. (2018) noted a similar overrun level
(8.76–15.31%) in ice cream composed from coconut milk, while Elsabie
and Aboel Einen (2017) observed 10% lower overrun for ice cream
based on nuts and sesame drink than for those based on cow milk.
Viscosity of ice cream mixes has a major influence on sensory quality
in general. The consistency coefficient (K) is a parameter which repre­
sents the viscous nature of ice cream. Correlation coefficient values for
adequate model ranged from 0.9996 to 0.9999, which can be satisfying
for analyzed ice cream mix samples and thus, the Herschel-Bulkley
model was selected to characterise the rheological behavior of all sam­
ples. The consistency coefficient values of classic milky ice cream has
been reported by different researchers, dependently on the level of
addition of various stabilizers, between 0.05 and 1.3 Pa sn (Aime,
Arntfield, Malcolmson, & Ryland, 2001; Minhas, Sidhu, Mudahar, &
Singh, 2002; Muse & Hartel, 2004). BahramParvar, Razavi, and Kho­
daparast (2010) determined the K coefficient for varying levels of food
gum such as CMC (carboxymethylcellulose) and concluded that for 0.5%
CMC addition the K value was as high as 6.822 Pa sn. In this research the
highest K value was noted for the sample without addition of stabilizers
(re) and it was 0.0373 Pa sn (Table 2), while with the addition of κ and
ι-carrageenan it was respectively 0.0013 and 0.0023 Pa sn (K mix and I
mix). The flow index (ni) in samples with stabilizers was lower than 1,
A. Kamińska-Dwórznicka et al. LWT 154 (2022) 112841

Fig. 2. Ice crystal size distribution in whey ice cream with LBG, guar gum and κ-carrageenan addition after different times of storage at − 18 ◦ C.

Fig. 3. Ice crystal size distribution in whey ice cream with LBG, guar gum and ι-carrageenan addition after different times of storage (24 h, 1 and 3 months)
at − 18 ◦ C.

Table 1 Table 2
Density, overrun, pH and melting time. Viscosity of whey ice cream sample at 25 ◦ C.
Sample Density [g/ Overrun [%] pH Melting time (first drop) Sample K [Pa sn] ni R2
cm3] [min] a
Re 0.0373 ± 0.51 0.1976 0.9999
x ± sd
K mix 0.0013c ± 0.14 0.7159 0.9997
Re 2.18a ± 0.48 12.91b ± 6.40a ± 18.25b ± 0.05 I mix 0.0023b ± 0.18 0.6315 0.9996
0.69 0.14
Explanatory notes.
K mix 2.62b ± 0.27 15.82c ± 6.44a ± 19.47c ± 0.05
re – reference sample (without any stabilizers), K mix – LBG plus guar gum with
0.30 0.32
I mix 2.60b ± 0.31 11.93a ± 6.39a ± 13.40a ± 0.05 the addition of kappa carrageenan.
0.17 0.24 I mix – LBG plus guar gum with the addition of iota carrageenan.
K – consistency coefficient, ni-flow index.
Explanatory notes. (x ±sd); a … c - mean values denoted by different superscripts differ statistically
re – reference sample (without any stabilizers), K mix – LBG plus guar gum with at p-value < 0.05.
the addition of kappa carrageenan.
I mix – LBG plus guar gum with the addition of iota carrageenan.
(x ±sd); a … c mean values denoted by different superscripts differ statistically at and we can infer non-Newtonian shear-thinning (pseudoplastic)
p-value < 0.05. behavior. It was found (Abbas Syed, 2018; Dłużewska et al., 2003) that
for whey mixes the viscosity and the K coefficient were lower than for
mixes without whey protein. Also it was reported that for hydrocolloids
such as κ-carrageenan gels there is lower force in the presence of whey

4
A. Kamińska-Dwórznicka et al.
Table 3
Comparison of ice crystals size distribution in whey ice cream samples after different storage times.
Time of Minimal size of ice crystals (μm) Maximal size of ice crystals (μm)
storage and
solution
variant
Re 24 h 12.43 78.91
1m 12.26 106.24
3m 17.66 120.65
K mix 24 h 6.26 38.73
3m 8.14 56.76
1m 11.17 62.66
I mix 24 h 3.13 33.60
3m 7.14 42.87
1m 9.55 46.13
Explanatory notes.
re – reference sample (without any stabilizers), K mix – LBG plus guar gum with the addition of kappa carrageenan, I mix – LBG plus guar gum with addition of iota
carrageenan.
protein than in milk systems (Mleko & Foegeding, 1999), because
α-casein molecule presents greater interaction with carrageenan’s,
resulting in an viscosity increase. This conclusion also suggests that the
synergistic effect between carrageenan and whey protein is a good goal
for further study.
Overrun and viscosity are closely related to the acidity of the ice
cream mixes. The higher potential acidity in the ice cream mix con­
tributes to the lower viscosity, which also reduces its overrun. The
structure of the ice cream after preparation becomes hard and heavy,
making the product undesirable (Markowska, Polak, Madaj, & Sadłow­
ska, 2019; Ruger, Baer, & Kasperson, 2002). In this study pH was
examined as a value strictly related to the acidity of the product. Based
on the results of the ANOVA test, stabilizer addition did not significantly
alter the pH of the ice cream mix compared to the sample without ad­
ditives (p-value > 0.05); (Table 1). It was reported (Lee & White, 1991;
Ruger et al., 2002) that ice cream mix pH lowered with increasing
addition of whey protein, 50% addition presented a pH of 6.42, while for
the control sample without addition of whey protein it was 6.57 (Lee &
White, 1991).
Melting time is an important qualitative feature for ice cream eval­
uation. It is determined by a number of factors such as: total solids,
overrun, acidity, number and size of fat particles, and finally size of the
ice crystals (Dłużewska et al., 2003; Góral et al., 2018), also the mix of
stabilizers should cause extension of melting time (Muse & Hartel,
2004). Góral et al. (2018) observed that with addition of inulin to co­
conut milk-based ice cream – inulin and LBG (in different proportions)
change the heat exchange conditions during ice cream production – a
decrease in cryoscopic temperature was observed, with a strong nega­
tive correlation as determined by Pearson’s correlation coefficient. They
also concluded that stabilizer addition influenced ice cream melting
time. Based on our results we can conclude that whey protein is also
involved in the melting process. Surprisingly, the shortest melting time,
13.4 min, was recorded for the sample with a mixture of LBG, guar gum
and ι-carrageenan as the stabilizing system, but it corresponded the
lowest overrun value for this sample. In the presence of calcium ions
usually this type of carrageenan easily creates a strong and durable gel
structure (Bui et al., 2019; Kaminska-Dworznicka et al., 2020; Wang
et al., 2020), it works more effectively in combination with LBG and is
more prone to syneresis. LBG forms a gel-like net and is dedicated to ice
creams containing animal protein also for ice cream systems rich in
polysaccharides (Góral et al., 2018). However, this combination in the
examined whey ice cream resulted in shortening of melting time (13.4
min), while for the sample with κ-carrageenan addition the longest time
was recorded 19.47 min and it was significantly different (p > 0.05)
from the melting time recorded for the control sample without any ad­
ditives (18.25 min). Carrageenan addition negatively influenced the
melting time of ice cream. Soukoulis (2008) reported that kappa
carrageenan used in milk ice cream instead of xanthan gum shortened
5
LWT 154 (2022) 112841
Average diameter DA in the class with the highest frequency (μm) ± standard deviation SD
58.15 ± 1.71
59.79 ± 1.52
68.18 ± 1.87
26.97 ± 1.72
34.66 ± 2.07
37.98 ± 1.98
20.91 ± 1.78
24.86 ± 1.91
28.02 ± 1.75
the melting time of the examined ice cream. Generally the melting time
of whey ice cream was shorter than the melting time found usually for
milk ice cream and the values were closer to the results obtained for
coconut ice cream in the research of Góral et al., 2018, which could be
related to the similar content of fat and polysaccharides. On the other
hand (Kot Anna, 2020) observed the melting time for ice cream based on
almond drink nearly 50% longer than in our research for the combina­
tion of LBG, xanthan gum and inulin as a stabilizing mix. For this sta­
bilizers combination longer ice cream melting time was noted for
concentrated fruit ice cream (Dłużewska et al., 2003).
3.2. Microscopy structure analysis
Large ice crystals have a negative effect on the textural properties of
the product. Table 3 clearly shows changes in the equivalent diameter of
ice crystals for whey ice cream samples with and without the addition of
LBG, guar gum and two variants of carrageenan. For the non-stabilized
sample and both examined stabilizing mixes it was discovered that in ice
cream without any addition average crystals diameter just after pro­
duction was 58 μm, while for the stabilized samples ice crystal average
diameters were respectively 27 and 21 μm, for the addition of kappa and
iota carrageenan (Table 3, Figs. 1–3). After one month of storage in the
non-stabilized sample X50 (ice crystals diameter at 50% of the cumula­
tive distribution function of the sample) was 35 μm and after 3 months of
storage it was 43 μm (Fig. 1). This result is lower than that observed in
milky ice cream without stabilization after one month of storage under
similar conditions. It was reported that even after one month of storage
in milky ice cream without stabilizers ice crystals could be larger than
50 μm (X50 parameter); (Flores & Goff, 1999; Lomolino, Zannoni,
Zabara, Da Lio, & De Iseppi, 2020). Sample without additives showed
the highest value for the consistency coefficient and this results corre­
sponds with the theory that recrystallization process is not strictly
related to the viscosity of the samples (Gaukel, Leiter, & Spieβ, 2014;
Leiter, Mailänder, Wefers, Bunzel, & Gaukel, 2017). In this research a
high amount of whey protein present in ice cream composition could
affect the appearance of the crystal structure. According to a study by
(El-Zeini, El-Abd, Mostafa, & El-Ghany, 2016), whey may contribute to
reduction of the size of ice crystals due to the fact that it causes better
dispersion of air bubbles. The thesis formulated in these studies is also
confirmed by a previous study (Chun, Kim, & Min, 2012). They also
claimed that with the increase in the amount of whey in ice cream
smaller ice crystals arise and recrystallize to smaller sizes with time. For
all of the variants it is obvious that the addition of hydrocolloids posi­
tively influences ice crystal diameters. When analyzing the ice crystal
diameter at 50% of the cumulative distribution of the sample (X50), it is
clear that for samples with additives, the smallest ice crystals were
created in whey ice cream with ɩ-carrageenan addition (Figs. 2 and 3)
and the X50 parameter even after 3 months of storage was at the level of
A. Kamińska-Dwórznicka et al.
23 μm while for κ-carrageenan addition it was 29 μm. This could also be
related to the fact that this sample was characterized by the lowest
overrun value and melted faster than the two other samples, since air
bubbles create an isolator preventing faster heat transfer. It was previ­
ously reported that ɩ-carrageenan with calcium ions (present in whey ice
cream) exhibits unusual thixotropic behavior and creates softer and
more resilient gels than with potassium salts (Bui et al., 2019). Calcium
is a divalent cation that has the ability to create intra-molecular com­
binations between the sulfate groups of approximal anhydro-D-galactose
and D-galactose of ɩ-carrageenan (Cosenza, Navarro, Ponce, & Stortz,
2017). Probably the whey protein with the combination of ɩ-carrageenan
creates a favorable structure with the best water holding capacity
resulting in better crystal structure creation. On the other hand Ji-Chun
et al. (2012) in their research on thermal properties and physical activity
of whey and κ-carrageenan found that with an increase in the proportion
of whey proteins with the participation of κ-carrageenan in ice cream,
the equivalent diameter of ice crystals decreases and after 72 h of stor­
age, the average crystal sizes of the ice cream were 71.15, 64.02 and
58.52 μm for respectively: 1.0, 3.0 and 5.0% of whey addition. For all of
the examined variants even after such a long period as 3 months the X50
parameter did not exceed 50 μm and it has been reported that this level
Fig. 4. Microscopic images of ice crystals in whey ice cream without stabilizers addition (re), with LBG, guar gum and κ-carrageenan addition (K mix) and with LBG,
guar gum and ι-carrageenan addition (I mix) after different time of storage (24 h 1 and 3 m (months)) at − 18 ◦ C.
6
LWT 154 (2022) 112841
is highly accepted for ice cream with good quality and desired texture.
Samples with added hydrocolloids showed smaller ice crystal sizes,
although with more uniform structure than samples without any addi­
tion (Fig. 4). Changes in the shape of ice crystals particularly visible in
the sample without any additives may suggest that coalescence between
adjacent crystals occurred (Fig. 4 re). Samples with the addition of
carrageenan’s (Fig. 4: K mix and I mix) presented smaller diameters of
crystals for both fractions however ice crystals in the sample with iota
carrageenan addition, were more regular with a fraction of very fine
round and small ones. The same shape of ice crystals was noted for
strawberry sorbets with iota carrageenan addition (Kamińska-Dwórz­
nicka et al., 2020). Kamińska-Dwórznicka et al. (2015 and 2020)
demonstrated also for strawberry sorbet with κ-carrageenan addition the
shape of ice crystals as more angular and elongated, which was also
similar for the examined whey ice cream. We can concluded that the
shape of ice crystals is strictly dependent on the type of added stabilizers
while the diameter is also influenced by the ice cream composition.
4. Conclusions
The ice cream based on whey protein was characterized by
A. Kamińska-Dwórznicka et al.
physicochemical properties and ice crystal structure analysis. It was
discovered that whey presence increases density and viscosity and re­
duces overrun of the analyzed product. Examined stabilizing mixes also
modified density (higher for the sample with additives), melting time
and overrun value. The lowest overrun value (11.93%) and simulta­
neously the shortest melting time (13.4 min) were recorded for the
ι-carrageenan addition. An unexpected high value of consistency coef­
ficient was noted for the sample without additives. No influence of
stabilizing systems on pH of tested ice cream was found.
The best in crystal growth inhibition was found for the stabilizing
mix containing ι-carrageenan for which after 3 months of storage
average ice crystal diameter was 28 μm while for the sample without
additives it was 68 μm. The shape of ice crystals was also influenced by
the stabilizing system. To summarize, it was found that it was possible to
prepare ice cream based on sweet whey using stabilizers applied in
traditional ice cream production. Organoleptic evaluation as well as
examination of lactose recrystallization should be the subject of further
investigation.
CRediT authorship contribution statement
Anna Kamińska-Dwórznicka: Conceptualization, Software, Vali­
dation, Investigation, and analysis of particular methods: Physico­
chemical properties of whey ice cream analysis, Microscopy structure
analysis, Writing – original draft, Writing – review & editing, Supervi­
sion. Sylwia Łaba: Conceptualization, and analysis of particular
methods: Physicochemical properties of whey ice cream analysis,
Writing – review & editing. Ewa Jakubczyk: Conceptualization, Soft­
ware, Validation, Investigation, and analysis of particular methods:
Physicochemical properties of whey ice cream analysis, Microscopy
structure analysis, Writing – review & editing, Supervision.
Declaration of competing interest
The authors have no affiliation with any organization with a direct or
indirect financial interest in the subject matter discussed in the
manuscript.
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