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Journal of Food Engineering 237 (2018) 215–225

Contents lists available at ScienceDirect

Journal of Food Engineering


journal homepage: www.elsevier.com/locate/jfoodeng

Cheese feed to powder: Effects of cheese age, added dairy ingredients and T
spray drying temperature on properties of cheese powders
Denise Felix da Silvaa,∗, Cosima Hirschbergb, Lilia Ahrnéa, Anni Bygvrå Hougaarda,
Richard Ipsena
a
Department of Food Science, Faculty of Science, University of Copenhagen, Rolighedsvej 26, DK-1958 Frederiksberg C, Denmark
b
Department of Pharmacy, Faculty of Health and Medical Sciences, University of Copenhagen, Universitetsparken 2, 2100 Copenhagen, Denmark
A B S T R A C T

The effects of cheese age and addition of dairy ingredients on cheese powder properties have not been previously investigated. Hence, the effect of addition 2%
sodium caseinate plus 2% buttermilk powder (B2S2) or 4% buttermilk powder (BMP) were evaluated. The addition of these ingredients led to a decrease of the Power
Law consistency index in cheese feeds made from 16 to 30 weeks old Danbo cheeses. Powders containing B2S2 presented homogeneous particle size distributions,
lower amount of free fat and better flowability, due to improved fat emulsification, confirmed by confocal laser microscopy. Powders with BMP presented higher
browning index, cohesiveness and spontaneous primary agglomeration. These powders were also more sensitive to an increased temperature difference (ΔT) between
inlet and outlet spray drying temperatures, causing more browning. Cheese powder properties could thus be significantly improved by addition of 2% SC plus 2%
BMP, whereas no improvements were observed using only BMP.

A R T I C LE I N FO

Keywords:
Cheese feed
Cheese powder
Flowability
Microstructure
Buttermilk powder
Sodium caseinate powder

1. Introduction 2014). Disodium hydrogen phosphate is an ES commonly used to im-


prove emulsification by Ca2+ binding, pH adjustment, casein solubili-
Cheese powders are produced by spray drying a mixture of minced zation and fat emulsification and, therefore assist the emulsion stabi-
cheeses, water and other ingredients such as emulsifying salts (ESs), lization up to spray drying (Lucey et al., 2011; Varming et al., 2014).
heated to form a homogeneous emulsion, termed cheese feed (Felix da Nonetheless, due to current requirements for reduction of the amounts
Silva et al., 2017; Hougaard et al., 2015; Kelimu et al., 2017). Cheese of sodium and phosphate in food, the development of cheese powder
feed is a concentrated emulsion-like system, where stability and flow with the reduced amount or without ES has been investigated
behavior are important properties for the further processing and final (Hougaard et al., 2015; Kelimu et al., 2017; Varming et al., 2014).
product quality of cheese powders. Many types of cheeses can be used Milk proteins have been largely utilized in the food industry as
to produce cheese powders e.g. Danbo, Emmental, Camembert and emulsifiers due to their amphiphilic nature. Therefore, they also have
Gouda. Danbo is a smear-ripened semi-hard Danish cheese variety with potential application in the improvement of emulsification in cheese
small round eyes (Antonsson et al., 2003) that has been widely used to feed without ES. Sodium caseinate (SC) is known for its high emulsi-
produce cheese powder in Denmark with different ripening time. fying capacity (Crowley et al., 2016; de Figueiredo Furtado et al., 2017;
It has been shown that cheese feed stability and flow behavior, as Dickinson, 2006; Lam and Nickerson, 2013). Furthermore, the protein
well as the powder properties, can be affected by many factors such as adsorption onto the interface can provide a combination of electrostatic
the use of different cheeses, and their composition and the addition of and steric repulsion between oil droplets (Wilde et al., 2004), which
ingredients (Hougaard et al., 2015; Kelimu et al., 2017; Varming et al., may allow formation of a stable cheese feed. Likewise, buttermilk


Corresponding author.
E-mail address: denise@food.ku.dk (D. Felix da Silva).

https://doi.org/10.1016/j.jfoodeng.2018.05.015
Received 18 March 2018; Accepted 14 May 2018
Available online 15 May 2018
0260-8774/ © 2018 Elsevier Ltd. All rights reserved.
D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

powder (BMP) has recently received increased attention as a functional protein) indicated the instability of the cheese feed. The height of water
ingredient and is mainly used as emulsifier due to its protein and milk phase in the tube was measured after 1, 2, 3, 4 and 5 min, which was
fat globule membrane content (Corredig and Dalgleish, 1998; Ihara used as an indicator of emulsion instability. Analyses were carried out
et al., 2011; Roesch et al., 2004). Buttermilk is a by-product from butter in triplicate for each cheese feed batch.
manufacture and contains water-soluble material such as phospholipids HAAKE RheoStress 600 (Thermo Fisher Scientific Inc., Karlsruhe,
caseins, minor peptides, whey proteins and lactose (Corredig and Germany) rheometer containing a stainless steel bob-cup geometry with
Dalgleish, 1998; Roesch et al., 2004). a rotating cone (d = 40 mm) was used to obtain the flow curves (shear
The physical and functional properties of cheese powders, such as stress versus shear rate). An aliquot of approximately 30 mL of cheese
powder flowability and rehydration properties, are affected by the feed was placed into the cup and submitted to an up-down shear rate
properties of the cheese feed, the use of different cheese raw materials, sweep from 0 to 300 s−1 with 4 mm gap at 50 °C. The flow curves were
the addition of ingredients as well as by spray drying and storage fitted to the Power Law model (Equation (1)) by nonlinear regression
conditions (Felix da Silva et al., 2018, 2017). However, the influence of using Origin Pro 9.1 (OriginLab Corporation, Northampton, MA 01060
cheese feed on the characteristics of cheese powders have not been USA).
widely studied, and most of the prior research has dealt with flavor
σ=Kγ̇ n (1)
aspects (Varming et al., 2013, 2011) or characterization of cheese
powder properties (Erbay and Koca, 2015; Felix da Silva et al., 2017, Where: K is the consistency coefficient (Pa·s ), n is the flow behavior
n

2018; Koca et al., 2015). index (-).


In this study, we aimed to understand how the use of Danbo cheeses
with different ages, and the addition of sodium caseinate and butter- 2.4. Cheese powder characterization
milk powder as ingredients, affected cheese feed behavior and conse-
quently the physical properties of the powder. In addition, the influence 2.4.1. Composition and water activity
of the temperature difference (ΔT) between inlet and outlet spray Lactose was measured using an enzymatic method (ISO 2002).
drying temperatures was also investigated. Correlations between cheese Furthermore, the pH of a solution of cheese powder in water (1:3) was
feed and cheese powder characteristics are discussed. determined using a digital pH-meter (Hach HQD, Loveland, Colorado,
US). The moisture and ash content was determined gravimetrically at
2. Materials and methods 105 ± 2.0 °C and 525 ± 25 °C, respectively. Fat was determined by
the Gerber method. Protein was quantified by Kjeldahl using a nitrogen-
2.1. Cheeses and dairy ingredients to-protein conversion factor of 6.38. All methods were as described by
Ardö & Polychroniadou (1999). Fat and protein of cheese feeds were
Smear-ripened Danbo (Them Ost, Them, Denmark) cheeses with quantified by Near-Infrared (NIR) spectroscopy using InfraXact™ Lab/
different ages (16, 30 and 45 weeks) and soft white cheese (Nordex Pro (Foss Analytical, Hillerød, Denmark). Free fat was quantified based
Food A/S, Dronninglund, Denmark) were used to produce cheese on the GEA Niro analytical method (Niro, 2005) for surface free fat with
powders. Sodium caseinate and sweet buttermilk powder were pur- modified quantities of powder (1.5 g) and petroleum ether (100 mL).
chased from Friesland Campina DMV (Amersfoort, The Netherlands) Water activity was measured by using an Aqua Lab 3 TE (Decagon
and Falköpings Mejeri (Falköping, Sweden), respectively. Devices, Inc., USA) at temperature 20 ± 1 °C.

2.2. Cheese powder manufacture 2.4.2. Color


Color parameters L (lightness), a (redness) and b (yellowness) were
Cheese powder samples were produced at pilot plant scale at measured with a Chroma Meter CR-400 (Konica Minolta Business
Lactosan A/S (Ringe, Denmark) by spray drying a mixture of melted Technologies, Inc., Tokyo, Japan). The colorimeter was standardized
smear-ripened Danbo (75% w/w) and soft white cheese (25% w/w) using the white calibration plate. Six determinations were performed
termed cheese feed. A one stage spray dryer (Anhydro Spray Dryer, SPX for each sample and results were expressed as average values. Hence,
Flow Technology, Søborg, Denmark) was used. Cheese feeds were browning index (BI) was calculated using L, a and b according to
prepared by cutting the cheeses and adding to a Stephan cooker equation (2) (Askari et al., 2008; Erbay and Koca, 2015).
(Stephan UMC5 electronic, Stephan u. Söhne GmbH, Hameln,
Germany) where water was added to ensure a dry matter in the cheese ⎛ ⎛⎡ (a + 1.75xL) ⎤⎞ ⎞
feed of 38 ± 1% (w/w), mixed for 5 min and heated up to 80 °C with ⎜100x ⎜⎢ 5.647xL + a − 3.012xb ⎥⎟ − 0.31⎟
⎝ ⎝⎣ ⎦⎠ ⎠
direct steam. Ingredients were added during cheese feed manufacture in BI =
0.17 (2)
powder form together with the cheeses and water prior to mixing and
heating. The pH of the feed was adjusted using potassium hydroxide Where L: lightness, a: redness and b: yellowness.
(KOH) to pH 5.9 ± 0.2. Cheese feed was sieved to remove unwanted
particles and then kept in a buffering tank for 30 min. Afterwards, it 2.4.3. Flowability
was homogenized at 10 MPa and then spray dried. The spray dryer Cheese powder flowability measurements were performed using a
settings were set to an inlet air temperature of 175, 185 or 190 °C and Schulze Ring Shear Tester (RST-Xs, Dr. Dietmar Schulze, Wolfenbüttel,
an outlet air temperature of 75 or 80 °C. The powder was cooled to Germany) with a pre-shear of 4 kPa and normal stresses of 1600, 2133,
20 °C, packed and stored at 4 °C prior to analysis. The experimental 2667 and 3200 Pa. A Type XS-Mr shear cell was used containing 30 cm3
design is described in detail in section 2.5. of cheese powder. The flow function coefficient (ffc) was calculated as
the quotient of the major consolidation stress and the unconfined yield
2.3. Cheese feed emulsion stability and rheological properties strength of the sample (Jenike, 1964; Schulze, 2010). Major con-
solidation stress is defined as the maximum normal stress undergone by
The stability of cheese feed emulsions was determined by a cen- a certain powder at a given state of compaction and the unconfined
trifugation method according to Hougaard et al. (2015) with mod- yield strength is defined as the cohesion within powder particles.
ifications. Aliquots of 30 mL cheese feed were filled into 50 mL poly-
propylene graduated tubes and centrifuged (300xg at 40 °C) using a 2.4.4. Particle size distribution (PSD)
Gerber centrifuge (Funke-Dr.N.Gerber Labortechnik, Berlin, Germany) Particle size distribution was determined using laser diffraction
for 5 min. The separation of the emulsion into phases (fat, water and (Mastersizer 3000, Malvern Instruments Ltd, Worcestershire, UK)

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

equipped with a dry powder disperser cell (Aero S). Approximately Three different cheese powder systems were investigated: a control
2.0 g of powder was placed in the feed hopper, with the feed pressure with no ingredient addition (NO), a formulation containing 2% (weight
set at 200 KPa. All measurements were taken at 0.5–2% obscuration by weight) buttermilk powder plus 2% (weight by weight) sodium
and the material refractive and absorption indices of 1.57 and 0.01, caseinate (B2S2) and a third system with addition of 4% (weight by
respectively (Felix da Silva et al., 2018). weight) buttermilk powder (BMP) on cheese feed wet basis. Those
formulations were chosen based on previous performed research
2.4.5. Particle microstructure of powders (Kelimu et al., 2017). Samples were coded according to their in-
The microstructure of cheese powders was evaluated using scanning gredients addition (NO, B2S2 or BMP) followed by the Danbo cheese
electron microscopy and confocal scanning electron microscopy. age (16, 30 or 45 weeks) and the temperature difference (ΔT = 100,
Scanning electron microscopy (SEM) was carried out using a FEI 105 or 110 °C) between inlet and outlet spray drying temperatures.
Quanta 200 scanning electron microscope (FEI Company, Hillsboro, Samples containing 4% of sodium caseinate was not suitable for cheese
USA) equipped with a back-scattered electron detector. Prior to analysis powder production once the feed was not homogeneous.
samples were attached to double-sided adhesive carbon tabs mounted Measurements were carried out in triplicates. Analysis of variance
on scanning electron microscopy stubs, coated with gold/palladium. (ANOVA) was carried out using the Origin Pro 9.1 (OriginLab
For the confocal images, an inverted SP5X (Leica Microsystems GmbH, Corporation, Northampton, MA 01060 USA) software followed by
Wetzlar, German) confocal laser scanning microscope was used. The Turkey's multiple comparison test (p ≤ 0.05). In addition, composition,
samples were dyed with Nile Red 0.01% in 1,2-propanediol, which color parameters and flow function coefficient data were analyzed by
stained the fat phase, and Fast Green FCF 0.001% in 1,2-propanediol principal component analysis (PCA) using the software LatentiX 2.0
which stained the protein. Illumination was provided by an Argon laser (LatentiX, Frederiksberg, Denmark).
at 488 nm and a Helium/Neon laser at 633 nm (Felix da Silva et al.,
2018). 3. Results and discussion

2.5. Experimental design and statistical analyses 3.1. Composition of cheeses

The cheese powder formulations, cheese age, and drying tempera- Table 2 shows the composition of the soft white cheese and the
ture difference, as well as their samples codes, are shown in Table 1. three Danbo cheeses used for the manufacture of cheese powders. No
significant differences (p ≤ 0.05) were found for the average values of
Table 1 moisture, fat, protein, ash and lactose content comparing the Danbo
Design of experiments (NO- No added Ingredient, BMP –buttermilk powder and cheeses of different ages. This also applied when the soft white cheese
SC – sodium caseinate and B2S2 (2% BMP +2% SC). was excluded from the statistical analysis. As expected, an increase in
proteolysis with aging was indicated by pH 4.6 soluble nitrogen values,
Sample code Cheese age Ingredient Inlet/outlet Temperature
temperature difference (ΔT) of
which may also explain the slight increase in pH for Danbo cheeses with
(°C) spray drying (°C) cheese aging.

NO_16_100 16 weeks NO 175/75 100 3.2. Rheological properties of cheese feeds


NO_16_105 NO 185/80 105
NO_16_110 NO 190/80 110
B2S2_16_100 2% BMP 175/75 100 The cheese feeds were evaluated regarding their chemical compo-
+2% SC sition, physical stability, and flow properties. The pH and moisture
B2S2_16_105 2% BMP 185/80 105 content was adjusted to 6.0 ± 0.4 and 60.0 ± 2.0% (data not shown)
+2% SC
as a standard procedure in cheese powder manufacture (Felix da Silva
B2S2_16_110 2% BMP 190/80 110
+2% SC et al., 2017). Fat (17.0 ± 1.0%) and protein (15.0 ± 1.2%) content of
BMP_16_100 4% BMP 175/75 100 cheese feeds did not differ significantly.
BMP_16_105 4% BMP 185/80 105 No phase separation was observed on the cheese feeds (data not
BMP_16_110 4% BMP 190/80 110 shown) before spray drying indicating a stable emulsion. The flow
NO_30_100 30 weeks NO 175/75 100
NO_30_105 NO 185/80 105
curves for the cheese feeds are presented in Fig. 1. The feeds with
NO_30_110 NO 190/80 110 different formulations showed differences in flow behavior (Fig. 1); an
B2S2_30_100 2% BMP 175/75 100 increase in cheese age decreased the viscosity of cheese feed, as ob-
+2% SC served from the slope of the curves, most likely due to the more de-
B2S2_30_105 2% BMP 185/80 105
graded protein in older cheese. At a given shear rate, higher shear
+2% SC
B2S2_30_110 2% BMP 190/80 110 stresses were found for feeds with no ingredient addition, while the
+2% SC addition of B2S2 led to a significant decrease of shear stress. The lowest
BMP_30_100 4% BMP 175/75 100 values were obtained with the addition of BMP. Within the same for-
BMP_30_105 4% BMP 185/80 105 mulation, (e.g. no added ingredients; NO) a decrease in viscosity was
BMP_30_110 4% BMP 190/80 110
NO_45_100 45 weeks NO 175/75 100
observed when more mature cheeses were used in the cheese feed. The
NO_45_105 NO 185/80 105 same decreasing behavior was found for formulation B2S2; however, in
NO_45_110 NO 190/80 110 this case, the differences were not as pronounced. For BMP feeds, no
B2S2_45_100 2% BMP 175/75 100 difference in flow curves was observed between Danbo cheese aged for
+2% SC
16 or 45 weeks. Feeds produced with 16 weeks old cheeses (Fig. 1A)
B2S2_45_105 2% BMP 185/80 105
+2% SC showed a greater hysteresis between up- and down sweeps, i.e. when
B2S2_45_110 2% BMP 190/80 110 the shear rate decreased the structure was not able to return to its pre-
+2% SC shear state immediately for the NO and B2S2 feeds, suggesting that the
BMP_45_100 4% BMP 175/75 100 structure was damaged by shearing and unable to recover its previous
BMP_45_105 4% BMP 185/80 105
BMP_45_110 4% BMP 190/80 110
structure. This behavior was not observed for BMP samples.
To characterize the rheological behavior of the cheese feeds, the
NO: without any ingredient addition; BMP: buttermilk powder; SC: sodium consistency coefficient (K) and the flow behavior index (n) were esti-
caseinate. mated from the Power Law model and are shown in Fig. 2. All samples

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Table 2
Composition of cheeses used in the formulation of the cheese feed.
Cheeses pH moisture (%) fat (%) protein (%) pH 4.6 soluble nitrogen (%) ash (%) calcium (%) lactose (%)

b b a a c a ab
Danbo 16 weeks 5.54 ± 0.07 45.4 ± 0.5 23.8 ± 0.8 24.3 ± 0.3 7.45 ± 0.80 3.70 ± 0.14 0.71 ± 0.02 0.03 ± 0.02a
Danbo 30 weeks 5.72 ± 0.06ab 45.8 ± 1.7b 23.8 ± 0.8a 24.2 ± 1.3a 8.75 ± 0.07b 3.80 ± 0.00a 0.66 ± 0.06b 0.08 ± 0.07a
Danbo 45 weeks 5.92 ± 0.07a 44.5 ± 0.3b 24.7 ± 0.4a 24.3 ± 0.6a 10.35 ± 0.21a 3.80 ± 0.14a 0.74 ± 0.00a 0.06 ± 0.03a
Soft white cheese 4.62 ± 0.08c 56.6 ± 3.0a 20.8 ± 3.9b 16.3 ± 1.5b 2.40 ± 0.98d 3.25 ± 0.07b 0.28 ± 0.00c 1.00 ± 0.84a

Means within a column with different superscripts are significantly different (p ≤ 0.05.

showed non-Newtonian shear-thinning behavior (n < 1), in which the 3.3. Cheese powder properties
apparent viscosity decreases with the increase of the applied shear rate.
A reduction in the viscosity during shearing of protein solutions can be 3.3.1. Composition of cheese powders
related to the spatial rearrangement of protein molecules in the liquid The composition of the cheese powders is shown in Table 3. All
and disruptions in their interactions; while in emulsions, shear-thinning powders presented similar fat, protein and ash content and moisture
can also be associated with flocculation of oil droplets (Drapala et al., lower than 2.4%. Even though the pH of cheese feeds was adjusted to
2017; Xu et al., 2012). More mature cheeses (45 weeks, i.e NO, B2S2, the same value prior to spray drying, a slight decrease in pH values as
and BMP) are likely to present a weaker protein network due to the the cheese age increased was observed for all formulations, especially
proteolysis during maturation, showing, therefore, higher values for the for BMP powders. This change may have occurred during the holding in
flow behavior index (n = 0.8–0.9) indicating a flow behavior closer to the buffering tank and might be related to an increase in buffering
Newtonian. capacity, as previously suggested by Hickey et al. (2017) with the ad-
A significant (p ≤ 0.05) decrease in the consistency coefficient, K, dition of 10% BMP in Cheddar style-cheeses. The authors identified a
was observed after addition of ingredients (B2S2 or BMP) especially to delay in the pH decrease upon maturation.
cheese feeds from 16 weeks old cheeses. The consistency coefficient, K, The lactose content was higher with the addition of BMP, which was
is indicative of the viscosity of the feed, but the comparison needs to be expected due to the high lactose content present in this dairy ingredient
done carefully due to differences in the flow behavior index (n) be- (51%). Sodium caseinate contains 88.0% of protein, 1.5% fat and 0.3%
tween the different feeds. Within the same formulation, increasing of lactose while buttermilk powder contains 33.0% of protein, 6.0% of
cheese age for formulations with no added ingredients (NO) and B2S2 fat and 51.0% of lactose. The free fat percentage was calculated based
caused a decrease in K value, whereas no significant difference on the amount of fat extracted from the total fat present in the powder.
(p ≤ 0.05) was observed with the addition of 4% BMP. In this context, free fat is considered the fat that is no longer emulsified
The effect of sodium caseinate (SC) and buttermilk powder (BMP), and it may be located at the powder particle surface and in pores and
as well as their combinations, on stability, fat droplet size and flow capillaries developed during the drying process (Kelly et al., 2014), thus
properties in cheese feed produced with Cheddar and soft white cheeses easily extractable. Free fat in dairy powders may be affected by powder
has previously been investigated (Kelimu et al., 2017). It was found that composition, homogenization pressure used in the feed, spray-drying
increasing the amount of SC in the cheese feed led to the formation of inlet/outlet temperatures and storage conditions (Kelly et al., 2014;
larger fat droplets, decreased viscosity and improved fat emulsification Vignolles et al., 2007). In this study, formulations containing 2% BMP
as well as improved physical stability. On the other hand, samples plus 2% SC (B2S2) showed the lowest amount of free fat, indicating a
containing only BMP presented smaller particles, exhibited instability better fat emulsification in the feed and within the powder particle. No
by phase separation (seen as creaming and protein precipitation). An significant differences were found between formulations NO and BMP.
appropriate cheese feed stability was found in samples with 2% SC plus Formulations with 30 weeks old cheeses exhibited the lowest amount of
2% BMP, which was attributed to both restructuring and emulsifying free fat for most of the powders. The presence of free fat in fat-rich
effects (Kelimu et al., 2017). powders can lead to issues during powder production such as powder
Similarly, in the present study, a decrease in viscosity of the feed cohesiveness, low yield, and production down-time as well as un-
due to the addition of SC and BMP, especially in 16 weeks old cheeses desirable final powder properties such as cohesiveness, caking, and low
may be associated with changes in fat droplet size. For Danbo cheeses, reconstitutability properties (Drapala et al., 2017; Kelly et al., 2014;
the BMP formulations presented the least viscous cheese feed, what Sadek et al., 2015). A similar reduction in the free fat content of cheeses
may be related to the presence of smaller fat droplets. It is likely in powder was previously observed by adding maltodextrin in the feed
concentrated emulsion systems, such as cheese feed, that the proteins (Erbay and Koca, 2015). The spray drying temperature difference (ΔT)
and phospholipids present in BMP will contribute to emulsifying the oil did not significantly influence the amount of free fat present in the
(Drapala et al., 2017; O'Mahony et al., 2017). cheese powders.

Fig. 1. Flow curves of cheese feeds. NO added ingredients (■), B2S2 ( ) and BMP ( ). Feeds produced with 16, 30 or 45 weeks old cheese are shown in A, B and C,
respectively.

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 2. Power Law model parameters of cheese feeds. NO added ingredients (■), B2S2 ( ) and BMP ( ). A shows the values of consistency coefficient K (Pa·sn) and B
shows the values of flow behavior index (n).

Table 3
Cheese powders composition.
Cheese pH moisture (%) fat (%) free fat (%) protein (%) pH 4.6 soluble salt (%) ash(%) lactose titratable water activity
powder nitrogen (%) acidity (%)
code

ΔT = 100 °C
NO_16 5.98 ± 0.10 2.1 ± 0.2 43.0 ± 0.5 84.4 ± 2.0 43.9 ± 0.7 10.3 ± 0.4 4.5 ± 0.1 8.2 ± 0.1 0.1 ± 0.0 2.2 ± 0.1 0.100 ± 0.00
NO_30 5.93 ± 0.12 1.6 ± 0.2 44.0 ± 0.3 81.0 ± 1.0 42.6 ± 1.0 12.3 ± 0.4 4.5 ± 0.1 8.0 ± 0.1 0.1 ± 0.0 2.2 ± 0.1 0.129 ± 0.01
NO_45 5.68 ± 0.15 2.2 ± 0.1 45.0 ± 0.2 81.6 ± 1.2 40.6 ± 1.2 14.0 ± 0.6 3.8 ± 0.2 7.2 ± 0.6 0.1 ± 0.0 3.0 ± 0.1 0.217 ± 0.01
B2S2_16 5.97 ± 0.10 1.9 ± 0.2 41.6 ± 0.5 78.9 ± 2.0 44.1 ± 1.0 10.1 ± 0.1 4.2 ± 0.1 8.2 ± 0.0 1.2 ± 0.0 2.3 ± 0.1 0.100 ± 0.00
B2S2_30 5.83 ± 0.10 2.1 ± 0.1 42.0 ± 0.5 77.4 ± ± 1.8 43.8 ± 0.5 11.5 ± 2.0 4.6 ± 0.1 7.6 ± 0.6 0.9 ± 0.0 2.5 ± 0.1 0.146 ± 0.00
B2S2_45 5.72 ± 0.14 1.8 ± 0.2 43.0 ± 0.5 76.0 ± 1.9 43.0 ± 0.5 13.4 ± 0.5 3.8 ± 0.1 7.2 ± 0.5 0.8 ± 0.1 3.1 ± 0.1 0.144 ± 0.00
BMP_16 5.60 ± 0.10 1.5 ± 0.0 42.8 ± 0.3 82.5 ± 1.6 42.1 ± 0.1 11.5 ± 0.7 4.3 ± 0.2 7.4 ± 0.3 1.8 ± 0.07 3.4 ± 0.1 0.178 ± 0.00
BMP_30 5.56 ± 0.10 1.2 ± 0.0 43.3 ± 0.4 82.21 ± 0.7 41.9 ± 0.1 12.0 ± 0.0 4.2 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.135 ± 0.00
BMP_45 5.50 ± 0.10 1.2 ± 0.0 43.2 ± 0.0 84.7 ± 0.3 42.2 ± 0.1 16.0 ± 3.4 4.0 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.100 ± 0.01
ΔT = 105 °C
NO_16 5.98 ± 0.10 1.2 ± 0.1 43.0 ± 1.0 87.2 ± 1.0 43.2 ± 0.7 10.0 ± 0.4 4.5 ± 0.1 8.2 ± 0.1 0.1 ± 0.0 2.2 ± 0.1 0.100 ± 0.00
NO_30 5.95 ± 0.12 1.6 ± 0.1 43.9 ± 0.3 83.6 ± 0.5 42.6 ± 1.0 11.2 ± 0.4 4.5 ± 0.1 7.9 ± 0.1 0.1 ± 0.0 2.3 ± 0.1 0.149 ± 0.02
NO_45 5.70 ± 0.15 1.4 ± 0.1 45.0 ± 0.2 87.8 ± 0.5 40.4 ± 1.0 14.0 ± 0.6 4.1 ± 0.4 7.8 ± 0.6 0.1 ± 0.0 3.0 ± 0.1 0.178 ± 0.02
B2S2_16 5.92 ± 0.10 1.6 ± 0.1 41.6 ± 0.5 77.4 ± 0.8 44.6 ± 0.5 9.9 ± 0.5 4.2 ± 0.1 8.1 ± 0.0 1.2 ± 0.0 2.4 ± 0.1 0.230 ± 0.01
B2S2_30 5.80 ± 0.10 1.9 ± 0.1 42.0 ± 0.5 80.0 ± 0.5 43.2 ± 0.5 10.0 ± 0.5 4.6 ± 0.1 8.2 ± 0.6 0.9 ± 0.0 2.5 ± 0.1 0.133 ± 0.00
B2S2_45 5.75 ± 0.14 2.1 ± 0.1 43.0 ± 0.5 85.0 ± 0.5 43.5 ± 0.5 10.3 ± 0.5 4.7 ± 0.1 7.5 ± 0.5 0.7 ± 0.1 3.0 ± 0.2 0.132 ± 0.01
BMP_16 5.56 ± 0.10 1.4 ± 0.1 42.8 ± 0.3 87.15 ± 0.7 42.1 ± 0.1 11.5 ± 0.7 4.3 ± 0.2 7.4 ± 0.3 1.8 ± 0.07 3.4 ± 0.1 0.116 ± 0.00
BMP_30 5.56 ± 0.10 0.9 ± 0.1 43.3 ± 0.4 81.4 ± 0.8 41.9 ± 0.1 12.0 ± 0.0 4.2 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.112 ± 0.00
BMP_45 5.53 ± 0.10 1.2 ± 0.1 43.2 ± 0.0 84.25 ± 1.3 42.2 ± 0.1 16.0 ± 3.4 4.0 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.115 ± 0.01
ΔT = 110 °C
NO_16 5.99 ± 0.10 2.4 ± 0.1 43.0 ± 1.0 85.1 ± 0.4 43.2 ± 0.7 10.0 ± 0.4 4.5 ± 0.1 8.2 ± 0.1 0.1 ± 0.0 2.3 ± 0.1 0.100 ± 0.00
NO_30 5.92 ± 0.12 1.5 ± 0.2 43.7 ± 0.3 83.6 ± 0.5 42.6 ± 1.0 11.2 ± 0.4 4.5 ± 0.1 7.9 ± 0.1 0.1 ± 0.0 2.3 ± 0.1 0.111 ± 0.00
NO_45 5.71 ± 0.15 2.1 ± 0.1 44.9 ± 0.2 86.9 ± 0.5 40.4 ± 1.0 13.2 ± 0.6 4.1 ± 0.4 7.8 ± 0.6 0.1 ± 0.0 3.0 ± 0.1 0.138 ± 0.00
B2S2_16 5.90 ± 0.10 2.1 ± 0.1 41.6 ± 0.5 83.7 ± 1.0 44.6 ± 0.5 9.9 ± 0.5 4.2 ± 0.1 8.1 ± 0.0 1.2 ± 0.0 2.3 ± 0.1 0.150 ± 0.00
B2S2_30 5.80 ± 0.10 2.3 ± 0.1 42.1 ± 0.5 78.3 ± 0.8 43.2 ± 0.5 9.9 ± 0.6 4.6 ± 0.1 8.2 ± 0.6 0.9 ± 0.0 2.5 ± 0.1 0.169 ± 0.00
B2S2_45 5.70 ± 0.14 1.7 ± 0.3 43.0 ± 0.5 76.0 ± 0.5 43.5 ± 0.5 9.9 ± 0.7 4.7 ± 0.1 8.0 ± 0.5 0.7 ± 0.1 3.2 ± 0.2 0.143 ± 0.00
BMP_16 5.55 ± 0.10 1.3 ± 0.1 42.8 ± 0.3 84.9 ± 0.8 42.1 ± 0.1 11.5 ± 0.7 4.3 ± 0.2 7.4 ± 0.3 1.8 ± 0.07 3.4 ± 0.1 0.116 ± 0.00
BMP_30 5.58 ± 0.10 1.0 ± 0.1 43.3 ± 0.4 79.7 ± 0.7 41.9 ± 0.1 12.0 ± 0.0 4.2 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.120 ± 0.00
BMP_45 5.53 ± 0.10 1.6 ± 0.1 43.2 ± 0.0 84.8 ± 0.7 42.2 ± 0.1 16.0 ± 3.4 4.0 ± 0.1 7.2 ± 0.1 1.8 ± 0.1 3.2 ± 0.1 0.147 ± 0.00
Dairy ingredients
SCa 6.5 6 1.5 – 88 – 1.65 4.5 0.3 –
BMPa 6.6 4 6 – 33 – – 8 51 –

a
Composition provided by the suppliers.

The water activity varied from 0.1 to 0.23 amongst the powders. 2015). The color of dairy powders is often related to Maillard reactions
However, the observed values are still acceptable for ensuring the (Gaiani et al., 2013) and the presence of lactose in BMP samples may
quality of spray dried powders. promote Maillard reactions and thereby result in higher browning
index. No effect of cheese age was observed for NO and B2S2 samples,
3.3.2. Color while for BMP the increase of cheese age concomitantly increased the BI
The browning index (BI) of cheese powders is presented in Fig. 3. BI value (Fig. 3), which might be explained by a combined effect of pro-
values of BMP samples were significantly higher at all three studied ΔT teolytic activity and presence of lactose.
values and consistently increased as the ΔT increased. This is in
agreement with a previous study that investigated the effect of outlet 3.3.3. Flowability
spray drying temperature in soft white cheese powders (Koca et al., Powders can be classified as not flowing, very cohesive, cohesive,

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 3. Browning index (BI) of cheese powdes. NO added ingredients (■), B2S2 (■) and BMP( ).

Fig. 4. Flow function coefficient (ffc) of cheese powdes. NO (■), B2S2 ( ) and BMP( ).

easy-flowing and free-flowing according to their flow function coeffi- exhibited lower ffc values, indicating a reduced flowability and a more
cient (Jenike, 1964; Schulze, 2010). Fig. 4 illustrates the flow function cohesive powder, however, a slightly higher value was observed when
coefficient (ffc) of cheese powders with different cheese age, in- 30 weeks old cheese and ΔT = 100 and 105 °C were used. The higher
gredients and ΔT of drying. The lower the ffc values the greater the cohesiveness of BMP powders may be related to the presence of
cohesion between particles. A ffc range of 1.31–1.78 was found for the amorphous lactose. Lactose in cheese powders has previously been
powders, which can thus be classified as very cohesive (1 < ffc < 2). found to be in the amorphous state caused by dissolution of the lactose-
In general, the difference between inlet and outlet spray drying tem- containing ingredient, i.e. sweet whey powder, in the cheese feed prior
perature (ΔT) of 100, 105 and 110 °C did not have a strong effect on to spray drying (Felix da Silva et al., 2018).
flowability. Powders without added ingredients made from 16 to 30 Significantly higher ffc values were found for formulations B2S2
weeks old cheeses tended to show higher ffc values than when in- and for 30 weeks old cheese. As previously reported by Fitzpatrick et al.
gredients were added, however, these differences may not be pro- (2007), the main factors affecting the cohesiveness of dairy powders are
nounced enough to be relevant in terms of application. BMP samples moisture, amorphous lactose, and fat content. The authors concluded

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 5. Cheese powders particle size distributions. A shows the powders produced with 16 weeks old cheeses and dried at ΔT = 100 °C; B shows the powders
produced with 16 weeks old cheeses and dried at ΔT = 105 °C; C shows the powders produced with 16 weeks old cheeses and dried at ΔT = 110 °C; D shows the
powders produced with 30 weeks old cheeses and dried at ΔT = 100 °C; E shows the powders produced with 30 weeks old cheeses and dried at ΔT = 105 °C; F shows
the powders produced with 30 weeks old cheeses and dried at ΔT = 110 °C; G shows the powders produced with 45 weeks old cheeses and dried at ΔT = 100 °C; H
shows the powders produced with 45 weeks old cheeses and dried at 45 weeks ΔT = 105 °C and I shows the powders produced with 45 weeks old cheeses and dried at
ΔT = 110 °C . NO added ingredients (■), B2S2:( ) and BMP( ).

that the powders with greater amounts of amorphous lactose were powders made using 45 weeks old cheese (NO and BMP) a significant
prone to caking, but the fat content on the particle surface influenced increase in particle size was observed. For BMP no effect of ΔT was
powder cohesiveness, with greater particle surface fat content resulting observed. The effect of cheese age and ΔT on PSD clearly depends on
in greater cohesiveness. Likewise, Kim et al. (2005) found that skim the formulation of cheese powders. For NO powders, using 45 weeks
milk powder had better flowability in comparison with fat-containing old cheese resulted in larger particle size, but ΔT did not affect sig-
powders (whole milk, cream, and whey protein powders) due to dif- nificantly. The combination of the added ingredients SC and BMP al-
ferences in surface composition. Similar behavior was found for fat- lowed the formation of particles with similar PSD regardless of the
filled spray-dried milk powder where the fat content has a major in- cheese age or drying temperature, however, the addition of only BMP
fluence on cohesiveness, with greater content resulting in greater co- samples resulted in larger particles and the higher the ΔT the larger the
hesiveness (Szulc et al., 2016). Thus, the better flowability found for particles for 16 weeks old cheese powders. Hence, particle size dis-
B2S2 powders may be related to the lower amount of free fat on the tributions were mainly affected by ingredients addition and cheese age,
surface (Table 3), while BMP powders, besides having a higher amount but to some extent, it was also affected when a higher drying tem-
of free fat, also contain lactose with a resulting greater contribution to perature was used, i.e. ΔT: 110 °C (B2S2_30 and NO_45).
the cohesiveness (decreased ffc values). Previous studies have shown that the viscosity of feed may affect the
spray dried powder particles size due to impaired atomization caused
by high viscosity. For milk protein concentrates, the feed with higher
3.3.4. Particle size distribution (PSD)
viscosity produced the largest particles (Crowley et al., 2014). Similar
The particle size distribution of cheese powders is presented in
behavior was observed for infant formula with different types of
Fig. 5. The particle sizes range from 20 to 1000 μm. In general, B2S2
emulsifiers; smaller particles were related to the feed having the lowest
powders showed smaller and more homogeneous particles seen as
viscosity (Drapala et al., 2017). However, for cheese powder, the par-
narrower peaks (20–150 μm). When 16 weeks old cheeses were used, a
ticle size distribution has shown larger particles for formulations with
slight shift to larger particles was observed for powders without added
lower viscosity (BMP). For these powders, this behavior may be related
ingredients (NO) dried using ΔT = 100 and 105 °C, but no difference
to their high cohesiveness (Fig. 4) which might cause a spontaneous
was found between NO and B2S2 when ΔT = 110 °C was applied. A
primary agglomeration during the spray drying process; therefore ag-
similar range (20–120 μm) of particle sizes were observed when 30
glomerates were measured as single particles in the particles size
weeks old cheese was used for NO and B2S2 formulations. However, for

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 6. Microstructure of cheese powders dried using ΔT = 100 °C visualized by scanning electron microscopy (SEM). A: NO_16; B: B2S2_16; C: BMP_16; D: NO_30; E:
B2S2_30; F: BMP_30; G: NO_45; H: B2S2_45; I: BMP_45. For abbreviation see Table 1.

distribution (Fig. 5). The high free fat together with the presence of emulsification in the feed implies a homogeneous distribution of fat
amorphous lactose could boost spontaneous primary agglomeration and within the powder particle. In this study, the interaction between fat
will be discussed in the next section. and protein differed depending on the ingredients as well as the cheese
age used for production. A better fat incorporation was observed for
feed B2S2 and a slight improvement was found for BMP powders
3.3.5. Microstructure compared to NO. Kelimu et al. (2017) have also shown that the addition
The microstructure of cheese powders was shown using both scan- of 2% SC plus 2% BMP in cheese feeds produced with Cheddar and soft
ning electron microscopy (SEM) and confocal laser scanning micro- white cheeses significantly improved the fat emulsification.
scopy (CLSM). No differences were observed in the microstructure of Likewise, the proteins present in the 30 weeks old cheese enables a
the powders with regards to the drying temperature; thus only micro- better emulsification, acting as a natural emulsifier. The extent of
graphs of samples dried using ΔT = 100 °C are presented (Fig. 6 and proteolysis during aging of cheese influences its functionality (Guinee
Fig. 7). Fig. 6 shows the scanning electron micrographs, which illustrate and Kilcawley, 2004), such as texture and meltability (Wang et al.,
the shape and structure of the powders. All powders presented spherical 2011). In this case, cheeses ripened for 30 weeks (pH 4.6 soluble ni-
and rough particles as previously reported for high fat containing trogen of 8.75 ± 0.07%) were able to promote a better fat emulsifi-
powders by (Schuck, 2009; Malafronte et al., 2015; Felix da Silva et al., cation in the cheese feed emulsion compared to 16 or 45 weeks cheeses
2017). The surface of dairy powder particles depend on the composi- for all formulations. Poor emulsification (as seen in NO samples) results
tion; high protein content powders present smoother surfaces, thus an in fat coalescence, thus the presence of lipid bridges between powder
increase in roughness is usually seen when the fat content increases. particles. This may lead to negative effects on the powder properties,
The main difference observed between the SEM images of the such as impaired rehydration properties (Fitzpatrick et al., 2016), faster
powders was the presence of smaller particles in the BMP formulations. lipid oxidation (Foerster et al., 2017) and greater cohesiveness (Szulc
The presence of free fat and lactose in these particles may have con- et al., 2016).
tributed to spontaneous primary agglomeration during spray drying,
observed as bigger particles in the particle size distribution measured
by laser diffraction (Fig. 5). This agglomeration often creates the ag- 3.4. Principal component analysis
glomerates of the type denoted ‘bunch of grape’ (Drapala et al., 2017).
Confocal laser scanning microscopy (Fig. 7) was used to visualize A principal component analysis provided an overview of the cor-
the fat and protein distribution within a powder particle. A good relations between the physical properties and how they were affected

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 7. Microstructure of cheese powders dried using ΔT = 100 °C visualized by confocal laser scanning microscopy (CLSM) where dark green color represents
protein and yellow color represents fat. A: NO_16; B: B2S2_16; C: BMP_16; D: NO_30; E: B2S2_30; F: BMP_30; G: NO_45; H: B2S2_45; I: BMP_45. For abbreviation see
Table 1.

by ingredient addition, cheese age and drying temperature (ΔT). The of the cheese feed (e.g. emulsification of the fat) due to the addition of
first two principal components (PC1 and PC2) explained 61% of the dairy ingredients or cheese proteolysis during maturation.
total variability. Four main clusters were found (Fig. 8A). Samples were Therefore, the rheological properties of the feed can be controlled
clearly separated according to their formulation, showing that the by selection of cheese age or addition of SC and BMP. The changes in
physical properties of cheese powders were affected by the addition of the composition of the feed have an effect on the final properties of the
ingredients and the cheese age. The main characteristics/properties of cheese powder and have therefore to be carefully selected. Cheese
the powders obtained from the different formulations were related to powder free fat, particle distribution and flowability can be sig-
flow function coefficient, salt content, and protein in group 2 (most of nificantly improved by the addition of ingredients that can improve the
B2S2 samples), while group 3 (BMP samples) was characterized by high emulsification of the feed such as 2% SC plus 2% BMP and/or using 30
browning and lactose content of the samples. Samples NO were divided weeks old cheeses. Addition of BMP has an effect on the powder color
into two groups (1 and 4), with the all 45 weeks cheese being clustered and cohesiveness observed by a reduced flowability and increased
in group 4 due to the high pH 4.6 soluble nitrogen, high fat content and particle size due to spontaneous primary agglomeration. The limited
free fat. Those correlations in combination with the obtained results improvement of flowability observed in this work may not be relevant
confirm the improvement in fat emulsification (reduced free fat) and from an industrial point of view, since cheese powders, in general, are
consequently the better flowability of B2S2 powders. In the same way, very cohesive powders.
BMP powders are clearly characterized by a high browning index as
shown in previous results. The differences observed when different ΔT
were used were not significant. Acknowledgments

We thank the Brazilian government's Science without Borders


4. Conclusions Program (National Council for Scientific Technological Development-
CNPq), the University of Copenhagen for financial support and Lactosan
This study demonstrated that the addition of two dairy ingredients, A/S. Cosima Hirschberg acknowledges the funding from Innovation
as well as the use of cheeses with different ages, can significantly in- Fund Denmark (Project: High-Quality Dry Products with Superior
fluence the composition and rheological properties of the cheese feed Functionality and Stability– Q-Dry, File No: 5150-00024B). The valu-
and consequently influence cheese powder properties, such as color, able cooperation of Inger Hansen, Heidi Oest, Ann Rasmussen and
particle size distribution, flowability, and microstructure. These dif- Danai Tziouri from Lactosan is gratefully acknowledged.
ferences can be explained by the changes in composition and structure

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D. Felix da Silva et al. Journal of Food Engineering 237 (2018) 215–225

Fig. 8. Principal component analysis on the composition and physical properties of cheese powders. Scores (A) and loadings (B) plots of PC1 versus PC2.

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