International Dairy Journal 123 (2021) 105162

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International Dairy Journal

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Rheology, microstructure and sensory properties of low-fat milk jam:

Influence of inulin type, sucrose content, sodium bicarbonate and
calcium chloride
E. Sulejmani a, O.S. Boran b, T. Huppertz c, d, A.A. Hayaloglu b, *
a
Department of Food Technology, University of Tetova 1200, Tetovo, Macedonia
b
Department of Food Engineering, Inonu University, 44280, Malatya, Turkey
c
FrieslandCampina, Amersfoort, the Netherlands
d
Wageningen University and Research, Wageningen, the Netherlands

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

Article history: We examined the effect of two types of inulin with combinations of sucrose, sodium bicarbonate and
Received 26 March 2021 calcium on the compositional, colour, rheological and sensory properties of low-fat milk jams (dulce de
Received in revised form leche). The two types of inulin had similar effect on the properties of milk jams, with some differences in
30 June 2021
consistency of the product. An increase in the storage and loss modulus and a decrease in flow behaviour
Accepted 5 July 2021
Available online 16 July 2021
of milk jams was observed after calcium addition. As sucrose content decreased, titratable acidity
decreased; however, ash and the colour values L*, a*, and b* increased. A negative correlation between
pH and L* (lightness) (P < 0.01) was found due to sodium bicarbonate used during production to support
the Maillard reaction. The results suggest that inulin can be used to improve the structure and rheo-
logical characteristic and sensory scores of the product with the combination of calcium.
© 2021 Elsevier Ltd. All rights reserved.

1. Introduction and added value to dairy products (Leddomado et al., 2021;

Milk jam, or dulce de leche, is a sweetened concentrated milk
product manufactured by the mixture of milk and sucrose, heated
under controlled conditions, generating a paste with a caramel
colour. It has a pleasantly sweet taste and it is used in the manu-
facture of bakery products, ice cream and confectionery products
(Silva et al., 2015; Zarpelon, Luciano, Andressa, Ribeiro, & Daguer,
2016). Based on the country where it is manufactured and traded,
this product is presented in different names and may vary in colour,
texture and flavour (Chaves, Souza, Colla, Bittenccourt, &
Matsushita, 2018; Vargas, Prestes, Miotto, & Prude ^ncio, 2021).
Recently, the product has become increasingly more popular in
Turkey, with the name of “milk jam”, or “süt reçeli” in Turkish, and
is consumed especially as a spread, dessert, and in ice-cream pro-
€
duction (Yüksel-Onür, 2018).
Several studies have been performed with the purpose of
partially replacing of the fat fraction, replacing (part) of the sucrose
and developing products using milk types to increase the aroma
* Corresponding author. Tel.: þ 90 422 377 4786.
E-mail address: adnan.hayaloglu@inonu.edu.tr (A.A. Hayaloglu).
Salvatore, Pes, Mazzarello, & Pirisi, 2014; Sołowiej et al., 2015). In-
vestigations on dulce de leche need to be supported to raise the
publication and commercialisation of such delicious product.
Knowledge of the processing conditions such as temperature, time,
pH, reaction kinetics that provide a desirable colour and a very
pleasant flavour to the product, rheology and variable of the pro-
cess of the formulations (the type and amount of neutraliser, the
composition of milk, the amount of sucrose) is directly related to
the quality of the resulting product (Rozycki, Buera, Piagentini,
Costa, & Pauletti, 2010; Stephani, Francisquini, Perrone, Carvalho,
& Oliveira, 2019; Zalazar & Perotti, 2011).
Inulin is one of the most well established and investigated pre-
biotics, which is accepted for food use without limitations and clas-
sified as food ingredients or food in all countries where it is used
(Guven, Yasar, Karaca, & Hayaloglu, 2005; Kolida, Tuohy, & Gibson,
2002). The degree of polymerisation (DP) represents the number of
monosaccharides of the carbohydrate chain and can influence various
properties of inulin, e.g., digestibility, prebiotic activity, sweetness, and
water-holding capacity (Pimentel, Garcia, & Prudencio, 2012).
Medium-length inulin represents a DP of 10, whereas long-chain
inulin (DP 23) is obtained by physical removal of short-chain mole-
cules (Cruz et al., 2013; Meyer, Bayarri, & Ta rrega, 2011). In reduced-fat

https://doi.org/10.1016/j.idairyj.2021.105162
0958-6946/© 2021 Elsevier Ltd. All rights reserved.
E. Sulejmani, O.S. Boran, T. Huppertz et al. International Dairy Journal 123 (2021) 105162

dairy products, inulin is often used as a fat-replacer and at a concen-
tration above 8%; long-chain inulin can display an identical creami-
ness and thickness in low-fat milk beverages compared with full-fat
milk beverages (Villegas, Carbonell, & Costell, 2007).
As the use of inulin as a fat replacer does not disrupt the casein
network, inulin can support the nutritional and technological ben-
efits of dairy foods (Guggisberg, Cuthbert-Steven, Piccinali,
Bütikofer, & Eberhard, 2009). Some investigation studied the effect
of the addition of inulin as supplements to physicochemical, rheo-
logical and sensory characteristics of dulce de leche and the fat
reduction in dulce de leche can lead to changes in the physico-
chemical characteristics, texture parameters, and sensory attributes
(Leddomado et al., 2021; Ranalli, Andres, & Califano, 2017).
Ramasubramanian, D'Arcy, Deeth, and Oh (2014) reported that the
addition of calcium chloride to pre-heated at 90  C milk for 10 min
enhances and influenced the structure development of strong milk
gels. Limited studies exist in the literature that evaluate, concomi-
tantly, the effect of adding long-chain and medium-chain inulin as a
fat replacer combined with calcium chloride on the physicochemical
and sensory properties of milk jam. Thus, the objective of this study
was to evaluate the influence of the addition of long-chain (GR) and
medium-chain (HP) inulin as a fat replacer combined with sodium
bicarbonate and calcium chloride on the rheology, physicochemical
properties and to assess the influence of descriptive attributes on
the sensory acceptance of the reduced-fat milk jam. In addition,
correlations between the L* values and pH were investigated for
possible prediction of changes in reactions relating milk jam colour.
mixture was kept at 100 ± 1  C for 15 min. After its cream like
consistency was obtained, the milk jams were divided into small
portions (approximately 150e200 mL) and stored at 4  C for
physical, chemical and sensory analysis. A total of sixteen batches
(see Table 1) of reduced-fat milk jam were manufactured in
duplicate.
2.2. Compositional analysis
The total solid content (%, w/w) of the samples was determined
gravimetrically by drying at 102 ± 1  C to constant weight. Protein
content (%, w/w) was determined by the micro-Kjeldahl method and
multiplied by 6.38 (Sulejmani, Sahingil, & Hayaloglu, 2020). Fat con-
tent (%, w/w) was determined by the Gerber method, as described by
Guven et al. (2005). Ash content (%, w/w) was determined gravi-
metrically after ashing of 3 g sample for 5e6 h in a furnace at 550  C.
Carbohydrate content (%, w/w) was calculated by difference, (i.e.,
carbohydrate (%) ¼ 100 e protein e fat e ash). Titratable acidity was
determined according to the alkaline titration method expressed as %
lactic acid (AOAC, 2005). The pH of milk jam was measured with a
Thermo Orion Prostar 4 model pH-meter in a mixture of 10 g sample
plus 10 mL of pure water, prepared with UltraTurrax T25 blender (IKA-
Werke GmbH, Staufen, Germany). Energy, in kcal per 100 g, was
calculated as ¼ (Fat  9) þ (Protein  4) þ (Carbohydrate  4), where
fat, protein and carbohydrate content were expressed per 100 g.
2.3. Colour analysis

2. Materials and methods The colour values of milk jam samples L* (brightness; 0e100), a*
(positive values redness; negative values greenness) and b* (posi-
2.1. Milk jam production tive values yellowness; negative values blueness) were analysed
using a Konica Minolta-Chroma Meter CR-5 as described in Bakirci,
UHT skimmed milk (0.15% fat) (4 L), (Migros, Malatya, Turkey), Dagdemir, Boran, and Hayaloglu (2017).
Inulin Orafti® GR and Inulin Orafti ® HP (BENEO, Mannheim Ger-
many), sodium bicarbonate (Dr. Oetker, Izmir, Turkey), sucrose 2.4. Rheological measurements
(Esenlik, Malatya, Turkey) and food grade calcium chloride were
commercially purchased from local markets. Production of Rheological analysis was performed using a Physica MCR 301
reduced-fat milk jam was carried out using the method described rheometer (Anton Paar GmbH, Ostfildern, Germany) with a Peltier
€
by Yüksel-Onür (2018) with some modifications. Two separate system for temperature control. Storage (G0 ) and loss (G00 ) modulus
trials were conducted with a week interval. The milk was heated and loss tangent (tan d) of the samples were obtained using a
with continuous mixing to a temperature of 100 ± 1  C and calcium 25 mm parallel plate (bottom plate was 35 mm in diameter, 1 mm
chloride (dissolved in water), sucrose and sodium bicarbonate were gap), by a frequency sweep (0.01e10 Hz) at 0.05% strain and 20  C
added at levels shown in Table 1. Inulin was also added and the (Bakirci et al., 2017). Specific attention was given to tan d, which
describes the ratio between G00 and G0 , where when tan d < 1
Table 1 (G00 < G0 ) elastic properties dominate and when tan d > 1 (G00 > G0 )
Ingredients for the production of low-fat milk jam.a gel-like or solid-state dominate (Jones, Brown, & Woolfson, 2001).
Treatment S (g) K (g) Ca (g) Inulin (g) Flow behaviour of the milk jam samples was assessed using the
same setup, whereby samples were first subjected to a shear rate of
GR HP
400 s1 for 180 s to break the characteristic hysteresis loop of
S100-GR 100 10
e e e
thixotropic fluids. Subsequently, samples were first subjected to
S100-HP 100 10
downward shear rate sweep, from 400 to 0.01 s1, followed by an
e e e
S100-K-GR 100 1.5 e 10 e
S100-K-HP 100 1.5 e e 10 up sweep from 0.01 to 400 s1. Experimental data were fitted to
S100-Ca-GR 100 e 0.735 10 e HerscheleBulkley model:
S100-Ca-HP 100 e 0.735 e 10
S100-K-Ca-GR 100 1.5 0.735 10 e s ¼ s0 þ K  ðg_ Þn
S100-K-Ca-HP 100 1.5 0.735 e 10
S50-GR 50 10
where s ¼ shear stress, s0 ¼ yield stress, g_ ¼ shear rate,
e e e
S50-HP 50 e e e 10
S50-K-GR 50 1.5 e 10 e K ¼ consistency index and n ¼ flow behaviour index. From these
S50-K-HP 50 1.5 e e 10 values, apparent viscosities (h at shear rate 50 s1, h50) at a fixed
S50-Ca-GR 50 e 0.735 10 e shear rate was taken.
S50-Ca-HP 50 e 0.735 e 10
S50-K-Ca-GR 50 1.5 0.735 10 e
S50-K-Ca-HP 50 1.5 0.735 e 10 2.5. Sensory and microscopy analysis
a
Abbreviations are: S, sucrose; K, sodium bicarbonate; Ca, 10 mM CaCl2; GR, 92%
inulin, 8% carbohydrate, 10% sweetness, 120 g 25  C solubility, 120 kcal; HP, 99.5%, Colour, external appearance, internal appearance, odour, con-
inulin, 0% carbohydrate, 0% sweetness, < 5 g 25  C solubility, 97 kcal. sistency (with a spoon), consistency (in mouth), spreadability,
2
E. Sulejmani, O.S. Boran, T. Huppertz et al. International Dairy Journal 123 (2021) 105162

sweetness, and general acceptability (9 point hedonic scale) were
evaluated by 10 trained panellists. While performing the sensory
analysis, the panellists were given water and bread to rinse their
mouth sensations between the samples.
For microscopy of the samples, an optical microscope (Leica,
model DM4000 M, Laser technik GmbH, Heidelberg, Germany) was
used for examination of the milk jam treatments with an oil im-
mersion objective (numerical aperture 1.4). Experiments were
done 3 images captured per 3 representative samples.
2.6. Statistical analysis
Two replicate trials were done for milk jam production and all
analyses were performed triplicate. Results were analysed by one-
way ANOVA using the SPSS package program (version 16.0). Dun-
can's multiple comparison test was used as a guide for paired
comparisons of treatment means. The level of significance of dif-
ferences between treatments was determined at P < 0.05.
3. Results and discussion
3.1. pH and composition of milk jam samples
Table 2 shows average values for total solids, ash, and energy as
well as the pH and titratable acidity (as a percentage of lactic acid)
of the samples. The typical composition of DL is a minimum 70%
total solids and 2% maximum for ash (Ferreira, Pimenta, Pinheiro,
Pereira, & Santos, 2011; Guimaraes, Leao, Pimenta, Ferreira, &
Ferreira, 2012; Perrone, Stephani, & Neves, 2011; Yüksel-Onür, € colour may occur. On the other hand, this characteristic is very
2018; Zalazar & Perotti, 2011); lower total solids contents were
found in the present study. The levels for lactic acid, total solid, and
ash contents in the milk jam samples ranged from 1.1 to 2.8%,
59.1e68.9%, and 1.7e3.0%, respectively, with a significant difference
between samples (P < 0.05). pH varied significantly between
samples from 6.22 to 6.80 (Table 2). The pH of the samples in the
present study were comparable with the data previously published
in the literature (6.0e6.8) reported by Gaze et al. (2015), Malec,
Llosa, and Vigo (1999) and Yüksel-Onür€ (2018). The addition of
calcium chloride, without sodium bicarbonate addition, to milk
induced a significant drop in milk pH (P < 0.05). Similar observa-
tions were made with calcium-induced gelation of milk during heat
treatment (Ramasubramanian et al., 2014).
The high moisture of the milk jams impairs the conservation of
the product, but a higher level of moisture in the product is known
to improve the sensory perception attributes (Demiate, Konkel, &
Pedroso, 2001). The moisture content did not show a significant
variation between the samples of the higher sugar added samples
group, but a significant difference between samples with lower
sugar content was apparent (P < 0.05). The moisture levels of milk
jam in the present study vary widely (from 32.2 to 40.9%). Demiate
et al. (2001), when analysing 42 samples of milk jams sold in Sa ~o
Paulo and Paran a, verified variations in the moisture content from
19.0 to 37.2% (w/w).
Colour parameters varied between the milk jam samples based
on the amount of sucrose and sodium bicarbonate used in product
preparation (Table 2). L*-values, which represent the lightness of
the product are higher than those reported for Argentinean dulce
de leche samples (Pauletti, Calvo, Izquierdo, & Costell, 1992). In
addition, L* values from the present study are somewhat higher
than the six commercial brands produced in Turkey (Yüksel-Onür, €
2018). Contrary to the investigation of Yüksel-Onür € (2018) we
found a negative correlation between pH and L* (r ¼ 0.661,
P < 0.01; Fig. 1) which may be due to the use of sodium bicar-
bonate in the formulations to increase pH and therewith the
extent of the Maillard reaction during production (Gime nez, Ares,
& G ambaro, 2008; Tuna & Arslan, 2016; Vargas et al., 2021).
Sample S50eKeCa-GR was found to differ significantly from the
other samples showing lowest b* parameters (Table 2) showing
strongly influences of light scattering affected by coagulation
(Fig. 2).
When dulce de leche is produced by a prolonged processing
time and/or by adding excessive neutralising agents, a darker
much desirable in dulce de leche used in ice cream manufacture
(Zalazar & Perotti, 2011). Furthermore, the lowest lightness and the
highest redness values of sample S100-K-HP (Table 2) indicates that
non-enzymatic browning reactions occurred at higher rates with
decreasing acidity (Perrone et al., 2011). Similar results were
€
attained by Yüksel-Onür (2018). It is known that there is the active
participation of the sucrose in the Maillard reaction, increasing the
tendency to browning (Oliveira, Penna, & Nevarez, 2009). Much
more intensive Maillard reaction at higher pH as in addition to
carbohydrates is from the deprotonated form of lysine that par-
ticipates in the Maillard reaction and the concentration of this in-
crease with increasing pH. The difference found in the colour
analysis, pH and the titratable acidity of the milk jam samples can
be induced by the manufacturing process and the raw material
used.

Table 2
Physico-chemical composition, energy values and colour properties of low-fat milk jam treatments.a

Treatments pH TA (%) TS (%) Ash (%) Energy (Kcal) L* a* b*

S100-GR 6.60 ± 0.01e 1.87 ± 0.19ef 68.3 ± 0.3c 1.83 ± 0.06 ab 254.5 ± 1.3d 47.6 ± 0.8d 0.98 ± 0.07cd 6.48 ± 0.33ef
S100-HP 6.60 ± 0.02e 1.99 ± 0.04f 68.0 ± 0.6c 1.70 ± 0.03a 252.8 ± 2.4d 49.6 ± 0.2de 1.34 ± 0.02b 6.13 ± 0.15e
S100-K-GR 6.81 ± 0.01ı 1.70 ± 0.15bcd 67.8 ± 0.3c 1.85 ± 0.02 abc 252.8 ± 1.4d 39.6 ± 2.0b 0.08 ± 0.29f 8.47 ± 0.47h
S100-K-HP 6.77 ± 0.01h 1.87 ± 0.00ef 68.6 ± 0.2c 1.91 ± 0.17 abc 254.4 ± 1.1d 35.3 ± 2.2a 1.11 ± 0.23g 11.31 ± 0.08ı
S100-Ca-GR 6.29 ± 0.01b 1.60 ± 0.09bc 68.2 ± 0.8c 2.19 ± 0.13cd 252.7 ± 3.1d 50.6 ± 0.1e 1.06 ± 0.10cd 7.28 ± 0.40g
S100-Ca-HP 6.22 ± 0.01a 1.12 ± 0.04a 68.9 ± 0.4c 1.80 ± 0.01 ab 255.8 ± 1.8d 51.0 ± 0.3ef 0.99 ± 0.05cd 8.94 ± 0.54h
S100-K-Ca-GR 6.64 ± 0.02f 1.58 ± 0.07b 68.2 ± 0.3c 2.13 ± 0.14 bcd 252.9 ± 1.1d 49.9 ± 0.3e 1.22 ± 0.16bc 3.78 ± 0.30abc
S100-K-Ca-HP 6.59 ± 0.03e 1.70 ± 0.11bcd 68.3 ± 0.4c 2.18 ± 0.10cd 252.3 ± 1.7d 49.9 ± 2.1e 1.12 ± 0.01bc 4.50 ± 0.23cd
S50-GR 6.54 ± 0.03d 2.59 ± 0.12gh 60.1 ± 0.4ab 2.19 ± 0.02cd 216.4 ± 1.9c 53.2 ± 1.2f 0.84 ± 0.12de 6.47 ± 0.69ef
S50-HP 6.53 ± 0.01d 2.83 ± 0.04ı 59.5 ± 0.7ab 2.14 ± 0.09 bcd 213.3 ± 2.5abc 56.6 ± 0.6g 0.69 ± 0.04e 7.57 ± 0.16g
S50-K-GR 6.74 ± 0.02g 2.48 ± 0.04g 59.5 ± 0.9ab 2.59 ± 0.08ef 212.7 ± 3.9abc 40.4 ± 0.3b 0.03 ± 0.23f 7.24 ± 0.71g
S50-K-HP 6.80 ± 0.00ı 2.48 ± 0.04g 60.4 ± 0.3b 2.69 ± 0.11efg 214.6 ± 1.7bc 42.5 ± 0.8c 1.18 ± 0.01bc 6.92 ± 0.27fg
S50-Ca-GR 6.38 ± 0.02c 2.70 ± 0.11hı 59.4 ± 0.2ab 2.41 ± 0.35de 213.2 ± 1.0abc 51.6 ± 2.2ef 2.06 ± 0.10a 4.30 ± 0.26bcd
S50-Ca-HP 6.39 ± 0.01c 1.76 ± 0.04cde 59.1 ± 0.8a 2.55 ± 0.05ef 209.9 ± 3.1a 53.1 ± 0.7f 2.08 ± 0.04a 4.96 ± 0.38d
S50-K-Ca-GR 6.65 ± 0.01f 1.69 ± 0.04bcd 59.3 ± 0.5a 2.95 ± 0.45g 210.6 ± 3.1ab 50.9 ± 0.5ef 2.05 ± 0.14a 3.08 ± 0.53a
S50-K-Ca-HP 6.61 ± 0.01e 1.82 ± 0.04de 59.5 ± 0.4ab 2.76 ± 0.35fg 211.0 ± 2.0ab 51.7 ± 1.2ef 1.92 ± 0.25a 3.66 ± 0.42ab
a
Abbreviations are: TS, total solids; TA, titratable acidity expressed in lactic acid. Values are means of 3 replicates; means in the same column that do not share a common
superscript letter are significantly different.

3
E. Sulejmani, O.S. Boran, T. Huppertz et al. International Dairy Journal 123 (2021) 105162

Fig. 1. Correlation between colour attributes (L*) and pH of low-fat milk jam samples (raw data and regression line).

Fig. 2. Appearance of low-fat milk jam samples.

4
E. Sulejmani, O.S. Boran, T. Huppertz et al.
3.2. Flow behaviour and dynamic oscillation rheology
Shear stress (s) against shear rate (g) was plotted for milk jams
with different ingredients (sucrose, CaCl2, sodium bicarbonate) are
depicted in Fig. 3. An increase in shear rate increased shear stress
rapidly and then levelled off as shear rate further increased
showing a characteristic behaviour of pseudoplastic fluids. The
yield stress (s0), flow behaviour (n) and the consistency (K) indices
were estimated by fitting the flow curves by the Herschel-Bulkley
model (Table 3). For six samples (S100-Ca-GR, S100-Ca-HP, S50-
HP, S50-Ca-GR, S50-Ca-HP and S50-K-Ca-HP), fitting the Hershell-
Bulkley model yielded poor fits and negative values for the con-
sistency index, K, which is physically impossible. Hence, no data for
the model parameters can be shown for these samples. For these 6
samples, visible coagulation was observed (Fig. 2). For the other 10
samples, the model of high values of coefficients of determination
(R2 > 0.99) were found when fitting the data. The consistency and
flow behaviour indices ranged from 1.4 to 39.4 Pa sn and 0.69 to
0.92, respectively (Table 3). All the investigated milk jam samples
were pseudoplastic fluids, but differed in their values of yield stress
(Table 3; Alimi, Mizani, Naderi, Mortazavian, & Moghadam, 2013;
Toneli, Park, Ramalho, Murr, & Fabbro, 2008).
Milk jam with code S100-Ca-HP sample was with greater vis-
cosity than the rest of samples displaying the highest h50 value
(apparent viscosity at shear rate 50 s1) meaning that HP inulin in
combination with calcium chloride enhances thickening proper-
ties. Less thixotropic behaviour resulted from higher structural
strength, indicated from the higher K value (Wani et al., 2013). Yield
stress can be defined as the lowest stress to start the flow and it
shows there may be interactions in the structure that must be
diminished before flow can commence. Comparable samples with
HP inulin had a significantly (P < 0.05) higher apparent viscosity
Fig. 3. Low-fat milk jam rheograms: a, ▪
S100-GR, S100-K-GR, : S100-Ca-GR, △ S100-K-Ca-GR GR; b,
S50-K-GR, : S50-Ca-GR, △ S50-K-Ca-GR; d, ▪
S50-HP, S50-K-HP, : S50-Ca-HP, △ S50-K-Ca-HP.
5
International Dairy Journal 123 (2021) 105162
than those with GR type inulin, while in milk jams with added
CaCl2 also showed higher viscosity than their counterparts without
added CaCl2 (Table 3). The effects of added CaCl2 on viscosity were
largely countered when sodium bicarbonate was added in combi-
nation with CaCl2. Similarly, previous findings suggested that only
low amounts of divalent cations are needed for aggregation
because they are effective in electrostatic interactions and their
ability to form salt bridges (Glibowski, 2009; Glibowski, Mleko, &
Wesolowska-Trojanowska, 2006).
Table 3 also shows the dynamic oscillation rheology properties
of milk jams and highlight significant differences in the G0 and G00
peak values. The maximal G0 value displayed significant changes
with the highest value of 190 kPa for sample S50-K-Ca-HP and the
lowest value of 1.7 kPa for sample S100-K-GR. With increasing
frequency, there was first a (somewhat more) rapid increase, after
which a linear relation was seen between frequency and G0 on a
log-log plots (Fig. 4). G0 was higher for samples with HP inulin than
for samples with GR inulin and for samples with CaCl2 addition
compared with those without added CaCl2, which may be due to
the effect of ionic calcium on the coagulation of milk protein during
heat treatment. In heated milk the evolution of heat-induced milk
gels may occur due to an increase in denatured protein induced by
an increase in clustering of the heat sensitive proteins. However, all
milk jams samples dominant elastic over viscous behaviour, since
G0 was greater than G00 and tan d which was <1. The calcium-
induced aggregation of protein and sucrose addition in milk
contribute to the high G'. The impact of heat treatment was pre-
viously shown on the physical properties of the calcium-induced
milk gels (Ramasubramanian et al., 2014). The final G0 values of
milk jams with sodium bicarbonate and calcium chloride were also
significantly (P < 0.05) lower than the final G0 values of milk jams
without added bicarbonate (Table 3).
▪ S100-HP, S100-K-HP, : S100-Ca-HP, △ S100-K-Ca-HP; c, ▪ S50-GR,
E. Sulejmani, O.S. Boran, T. Huppertz et al. International Dairy Journal 123 (2021) 105162

Table 3
Storage modulus (G0 ), loss modulus (G00 ), tan d, complex viscosity (ƞ*), and Herschel-Bulkley model parameters for low-fat milk jam treatments.a

Treatments G0  102 (Pa) G0  102 (Pa) Tan d h*  102 so (Pa) K (Pa sn) n R2 h50
S100-GR 108a 46a 0.43fg 186a 81.12a 39.40a 0.89a 0.9999 29.58d
S100-HP 47a 25a 0.53h 85a 2.21b 5.76b 0.90a 0.9998 3.98 abc
S100-K-GR 17a 10a 0.55h 32a 2.92b 6.94b 0.76bc 1.0000 2.80abc
S100-K-HP 25a 13a 0.55h 45a 12.43b 15.33b 0.79b 0.9999 6.55abc
S100-Ca-GR 1042b 225b 0.22a 1696b e e e e 25.87d
S100-Ca-HP 1251c 324c 0.26b 2056c e e e e 48.60e
S100-K-Ca-GR 53a 21a 0.41ef 91a 0.82b 1.43b 0.92a 1.0000 1.07a
S100-K-Ca-HP 80a 28a 0.35cd 135a 12.63b 4.45b 0.86a 0.9996 2.79abc
S50-GR 86a 33a 0.38de 146a 7.23b 4.00b 0.71c 1.0000 1.74ab
S50-HP 82a 32a 0.39e 140a e e e e 8.71abc
S50-K-GR 49a 22a 0.46g 86a 11.06b 15.07b 0.69c 1.0000 4.19abc
S50-K-HP 39a 20a 0.52h 70a 7.61b 13.19b 0.75bc 1.0000 5.00abc
S50-Ca-GR 863b 240b 0.28b 1425b e e e e 13.20bc
S50-Ca-HP 1233c 398d 0.32c 2061c e e e e 14.10c
S50-K-Ca-GR 18a 6a 0.33c 31a 2.77b 4.22b 0.71c 1.0000 1.51ab
S50-K-Ca-HP 1898d 529e 0.28b 3135d e e e e 1.48ab
a
Abbreviations are: G0 , storage modulus, at 0.1 Hz; G00 , loss modulus at 0.1 Hz; tan d ¼ G0 /G0 ; h*, complex viscosity; n, flow index; K, consistency index; R2,
coefficient of determination; h50, apparent viscosity at 50 s1. Values are means of 3 replicates; means in the same column that do not share a common superscript letter are
significantly different.

▪
Fig. 4. Storage moduli of low-fat milk jam as function of frequency at 20  C: a, S100-GR, S100-K-GR, : S100-Ca-GR, △ S100-K-Ca-GR; b, ▪ S100-HP, S100-K-HP, : S100-Ca-HP,
△ S100-K-Ca-HP; c, ▪ S50-GR, S50-K-GR, : S50-Ca-GR, △ S50-K-Ca-GR; d, ▪ S50-HP, S50-K-HP, : S50-Ca-HP, △ S50-K-Ca-HP.

3.3. Sensory evaluation and microscopy of the samples
Results from sensory evaluation and microscopic evaluation of
milk jam samples are given in Figs. 5 and 6. In terms of structure
and taste, only samples S100-HP, S50-K-HP and S100-K-HP were
found to differ significantly from the other samples (P < 0.05); for
appearance, texture and taste the S100-Ca-HP sample got the
lowest values (data not shown). The removal of milk fat and use of
6
sodium bicarbonate provided a positive effect on colour in sensory
test and use of inulin did not cause any change in colour. The colour
of milk jams treatments with added bicarbonate tended to be
preferred compared with similar samples treatments without bi-
carbonate (Fig. 6), which supports the desirable characteristics of
the product (Tuna & Arslan, 2016; Zalazar & Perotti, 2011). The
appearance of milk jam treatments containing higher sucrose
content perceived higher sensorial scored (Fig. 6), which may be
E. Sulejmani, O.S. Boran, T. Huppertz et al. International Dairy Journal 123 (2021) 105162

Fig. 5. Micrographs of low-fat milk jam samples (A: S100-K-GR; B: S100-K-HP; C: S100-K-Ca-GR; D: S100-K-Ca-HP).

Fig. 6. Sensory evaluations of low-fat milk jam samples.

related to Strecker degradation products promoting the formation HP inulin provided higher scores in generally acceptable, consis-
of a furan derivatives becoming 5-hydroxymethylfurfural tency and spreadability when compared with GR inulin (Fig. 6). In
(Damodaran, Parkin, & Fennema, 2010). Samples with HP inulin general, addition of HP inulin to the milk jams induced an increase
were perceived to be more acceptable on sensory evaluation and in consistency (to spoon and mouth), spreadability, softness and

7
E. Sulejmani, O.S. Boran, T. Huppertz et al.
overall acceptance for milk jams with sodium bicarbonate espe-
cially in the case of samples S100-K-HP, S100-K-Ca-HP and S50-K-
HP. Milk jams made with sodium bicarbonate were visibly more
homogenous and smooth (Fig. 2), which is because of the neu-
tralising impact and its effect on heat stability of the protein. When
reduced-fat samples were compared, these were preferred and
scored higher points by panel members than the full-fat counter-
parts [control sample (T) was tested for only in sensory evaluation
and given its formula as whole milk plus sucrose]. Lowering in
consistency and spreadability in reduced fat samples (by reducing
fat) was substituted by inulin. Sensory scores for inulin added and
control samples were almost the same in terms of appearance and
internal structure. On the other hand, sweetness scores were
almost the same in full-fat and reduced-fat milk jam samples.
However, addition of CaCl2 showed lower scoring in appearance,
internal structure, sweetness and also odour.
Gels made with calcium addition had large homogeneous pro-
tein clusters with no pores at scale bar 50 mm, while at scale bar
200 mm had spongier structure. It was previously reported that the
presence of inulin stabilises protein structure by developing a
second network that is not visible in confocal laser scanning mi-
croscopy (Guggisberg et al., 2009; Kip, Meyer, & Jellema, 2006).
Similarly, Glibowski and Glibowska (2009) found that a formed
calcium-inulin-protein structure is less porous than in Ca2þ-
induced protein and more compact than in inulin gel. In our case
only small deviations were noticed in the microstructure of treat-
ment containing two types of inulin (GR and HP) with added cal-
cium (Fig. 5). However, the results of microscopic investigations
support the influence of the type of inulin and calcium addition on
rheological characteristic, textural and sensorial properties
(Sołowiej et al., 2015).
4. Conclusions
Our results showed that the combination between calcium
chloride and HP inulin improves significantly the rheological
properties of milk jams and final G0 values, respectively. According
to the amount of sucrose and sodium bicarbonate used in pro-
duction, the lightness values are improved. It has been marked that
particular processing factors can impact milk jams sensory,
compositional and physical-chemical properties consequently,
knowing the product's rheology is relevant in improving compre-
hensive quality products. The difference in physicochemical char-
acteristic was greatly determined by the composition and structure
of the casein-calcium protein-inulin matrix. Overall, the investi-
gation improvement in rheological and structural properties,
manifested by higher storage and loss moduli recommend that HP
type inulin with calcium can be used as a possible fat replacer in
low-fat milk jam treatments.
Declaration of competing interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
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