Journal of Food Engineering 152 (2015) 8–16

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Journal of Food Engineering

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

Novel hydrothermodynamic food processing technology

Alex Martynenko a,⇑, Tessema Astatkie a, Varvara Satanina b
a
Dalhousie University, Faculty of Agriculture, Truro, Nova Scotia B2N 5E3, Canada
b
P.E.I. Berries Ltd., Montague, Prince Edward Island C0A 1R0, Canada

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

Article history: A novel hydrothermodynamic (HTD) technology for simultaneous crushing, homogenizing and pasteur-
Received 26 June 2014 ization of whole food in a turbulent flow as a single-unit operation was developed. The HTD technology is
Received in revised form 14 September based on the phenomena of high turbulence and cavitation in viscous liquids. HTD differs from hydrody-
2014
namic (HD) cavitation because it fully utilizes heat generated in the turbulent flow for product pasteur-
Accepted 1 November 2014
Available online 3 December 2014
ization. Pilot-scale HTD processing of whole blueberry resulted in homogeneous suspension with 13%
solids, 1.45–2.76 Pa s viscosity, stable texture and low sedimentation. HTD processing minimized effect
of thermal degradation of bioactive phenolics and increased shelf-life of pasteurized blueberry food.
Keywords:
Whole blueberry
Pasteurization at 95 °C provided <10 CFU/g microbial load, which was satisfactory for long-term storage.
Polyphenols This research proved the potential of HTD technology for manufacturing of innovative natural whole
Anthocyanins foods with high nutritional and nutraceutical values.
Viscosity Ó 2014 Elsevier Ltd. All rights reserved.
Rheology
HTD

1. Introduction in particular, high pressure processing (HPP), pulsed electric field

Global demand for health promoting foods with high nutri-
tional and nutraceutical values is increasing (Bagchi, 2008). It is
estimated that by 2020, the global market for whole and functional
foods will reach US $800 billion (Drouin and Gosselin, 2002). This
trend requires the development of novel minimal processing tech-
nologies. Most of conventional food processing technologies are
based on contact heating and involve multiple processing steps
that introduce fruit to the atmosphere and therefore accelerate
oxidation. Although high temperature short time (HTST) pasteuri-
zation and ultra-high temperature (UHT) sterilization could reduce
effect of oxidation due to decreasing time of exposure (Lozano,
2006), they are successfully used only for low-viscosity foods, like
milk and fruit juice, but not very efficient for processing of viscous
foods, like thick juice, sauce or puree.
‘‘No additives and preservatives ‘‘and ‘‘pure natural’’ food con-
cepts led to the development of novel technologies that are able
to keep food safe and fresh with minimal thermal processing. Sev-
eral non-thermal processing techniques were recently introduced;
Abbreviations: FBDG, Food Based Dietary Guidelines; C3G, cyaniding-3-gluco-
side; GAE, gallic acid equivalent; HD, hydrodynamic; HPP, high pressure processing;
HTD, hydrothermodynamic; HTST, high temperature short time; ORAC, oxygen
radical absorbance capacity; PEF, pulse electric field; UHT, ultra high temperature;
US, ultrasonic.
⇑ Corresponding author. Tel.: +1 902 893 6696; fax: +1 902 893 1406.
E-mail address: alex.martynenko@dal.ca (A. Martynenko).
(PEF), ultrasonic and irradiation (Knorr et al., 2011). HPP is the fast-
est developing option that emerged in food processing in the last
5–10 years. In HPP, food in sealed container is subjected to a high
hydrostatic pressure over time, which inactivates most of microor-
ganisms and prevents oxidation (Briones-Labarca et al., 2011;
Vázquez-Gutiérrez et al., 2011; Oey et al., 2008). More than 100
food companies around the world have already implemented
HPP to produce premium juices and other products with unique
functional and nutritional properties. Another alternative is PEF
technology with short high energy electric pulses, resulting in elec-
tric shock waves in the liquid that damage cell membranes
(Martín-Belloso and Soliva-Fortuny, 2011). However, it was
acknowledged that PEF could not provide food sterilization that
is often required for industrial applications (Lelieveld et al.,
2001). The same conclusion was made about ultrasonic, which
could provide partial microbial inactivation only in combination
with thermal treatment (Chandrapala et al., 2012). Food irradiation
partially destroys harmful pathogens by damaging proteins and
DNA; however, there is concern on the food safety after exposure
to radiation (Junqueira-Goncalves et al., 2011). All these novel
techniques share common characteristics, in particular very high
energy inputs that damage foodborne pathogens, which will also
increase the cost of processing.
Yet another underexplored food processing technology is
hydrodynamic (HD) cavitation (Gogate, 2011). Cavitation is
defined as the phenomenon of the formation, growth and collapse

http://dx.doi.org/10.1016/j.jfoodeng.2014.11.016
0260-8774/Ó 2014 Elsevier Ltd. All rights reserved.
 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16
of cavities occurring over an extremely small interval of time (mil-
liseconds), releasing large magnitudes of energy at the location of
transformation (Rayleigh, 1878). It was assumed that cavitation
on the microscopic level is accompanied by high pressure and tem-
perature gradients in the range of 100–5000 bar and temperature
gradients in the range of 1000–10,000 K (Suslick, 1990). However,
this assumption was not experimentally proven with direct mea-
surements. On the macroscopic level cavitation is characterized
by a dimensionless cavitation number Ca. This number expresses
the relationship between the pressure gradient and kinetic energy
per volume, indicating the potential of the flow to cavitate
(Batchelor, 1967):
p  pv
Ca ¼
0:5qV 2
where p is pressure of the liquid, pv is a vapor pressure, q and V are
density and characteristic velocity of the moving liquid.
According to Eq. (1), cavitation number is mostly determined by
the flow velocity and pressure gradients. Usually, cavitation occurs
at Ca 6 1 with the best operational conditions in the range of 0.1–1
(Gogate, 2011). Cavitation requires the low pressure and high
velocity of the moving liquid. Minimum flow velocity, causing
cavitation, is calculated as:
rffiffiffiffiffiffiffiffiffiffiffiffiffiffi
p  pv
V¼
0:5q
Energy, dissipated in the process of cavitation, is calculated from
the pressure drop Dp (Winter, 1987):
E ¼ Q  Dp
Due to the effect of high energy inputs on microbial cells dis-
ruption, HD cavitation could be used for food pasteurization
(Arrojo et al., 2008; Milly et al., 2007). However, mechanical
erosion of contact surfaces is the challenge for HD applications in
industrial settings. For example, cavitation in high-shear blenders
leads to quick wearing of moving parts (Chatterjee and Arakeri,
1997). Vortex cavitation addresses the problem of mechanical ero-
sion by focusing turbulence/cavitation in the center of the stream.
Shear forces are due to liquid–liquid friction, which minimizes fric-
tion on the interface. Due to the viscous dissipation, cavitation
energy is directly converted into heat. The average temperature
increase for adiabatic pipe flow is calculated from equation
(Winter, 1987):
Dp
DT ¼
qc p
Heat, generated on the microscopic level, provides volumetric
heating due to the mechanism of diffusion. High velocity and
turbulence of the flow, circulating in closed loop, facilitate heat
transfer. As a result of forced heat diffusion in turbulent flow,
thermal energy is distributed uniformly in the stream within sec-
onds. The entropy of moving liquid is increasing. This combined
effect of cavitation and volumetric heating in the moving liquid
could be defined as hydrothermodynamic (HTD) effect. However,
to our knowledge, there is no research on the synergetic effect of
cavitation and heat on biochemical, physical and microbiological
properties of foods.
This research aims to fill this gap in knowledge. The effect of
novel HTD technology on food properties was evaluated using wild
blueberries, which are rich source of bioactive phenolics, such as
anthocyanins, flavonoids and phenolic acids with health-promoting
effects (Wu and Prior, 2005; Basu and Lyons, 2012). Most of them
are located in the fiber matrix (Parada and Aguilera, 2007) and
could not be extracted in juice cold pressing (Satanina et al.,
2014). At the same time, bioactive phenolics are very sensitive to
9
matrix disintegration. Once fruit is crushed, the enzyme polyphe-
nol oxidase (PPO), initially separated from vacuolar phenolics in
intact cell, becomes available for phenolic oxidation. Temperature
is another significant factor of polyphenol degradation. Negative
effect of thermal processing on blueberry phenolics was reported
by Skrede et al. (2000), Lee et al. (2002), and Brownmiller et al.
(2008). For example, Lee et al. (2002) reported 87% anthocyanin
degradation in clarified pasteurized juice; and Satanina et al.
(2014) reported only 43% retention of anthocyanin in thermally
processed berries compared to 81% retention in berries processed
using the HTD technology. Heat accelerates chemical and enzy-
matic oxidation, which is perceived as a problem in manufacturing
health promoting fruit-based foods with acceptable shelf life
ð1Þ (Srivastava et al., 2007).
The hypothesis of this research was that simultaneous crushing,
agitation and heating of whole blueberries would release bioac-
tives from the matrix, while reduced oxygen environment would
protect them from oxidation. To test this hypothesis, we evaluated
effects of HTD processing on the quality and shelf-life of processed
blueberry.
2. Materials and methods
2.1. Experimental apparatus
ð2Þ
Food processing was done using a pilot-scale HTD processor,
initially designed for crushing and dispergation of plant seeds
(Osipenko, 2008). The physical principle of HTD is based on phe-
ð3Þ nomena of high turbulence and cavitation in viscous liquid (Fig. 1).
High turbulence in active area (cavitation zone) was created
due to a number of parallel bypass pipes of a smaller cross section
(nozzles), adapted to take the liquid from the mainstream and
return it back as a disturbing stream (Osipenko, 2008). Liquid at
high velocity enters cavitation zone, where the disturbing streams
induce local turbulence that generates multi-phase cavitation bub-
bles (nuclei). In this way, cavitation is focused on the center of the
stream, preventing erosion of metal surfaces. Further growth of
cavitation nuclei occurs downstream due to the pressure drop at
the orifice. Big bubbles are unstable and collapse right after going
through the active area of the cavitator. The quick collapse of the
cavitation bubbles creates local shear forces and releases energy
for crushing, homogenizing and heating of the fluidized product.
The primary advantage of HTD for whole food processing is volu-
metric heating, leading to uniform product pasteurization and
ð4Þ thermal inactivation of enzymes. Single-unit operation minimizes
product deterioration by excluding multiple processing steps. A
prototype of pilot-scale HTD processor (Tekmash, Ukraine) is
shown in Fig 2. It consists of the tank (1), electric motor (2), centrif-
ugal pump (3), pressure gauges (4), temperature sensors (5),
cavitator (6) and pressure relief valve (7).
The pilot-scale processor was designed for batch operation. The
capacity of the processor, including free volume of tank and pipes,
was 5.5  103 m3. Three-phase AC electric motor (2.2 kW,
1500 rpm) was connected to centrifugal pump. The pump with
outlet pressure of 1.41 MPa provided circulatory motion of the
liquid product with flow rate of 0.5  103 m3/s (Osipenko and
Lesnikov, 2009). With 38 mm diameter of main pipe, velocity of
the liquid was 0.45 m/s, reaching 1.5 m/s in the active area of cav-
itation. Reynolds number depended on product viscosity and
velocity. For liquid blueberry, it was in the range from 0.52 to
0.92  105, reaching 6.5  105 in the active area of cavitation.
Due to the high turbulence, mechanical energy of the stream was
converted into heat and accumulated in a form of thermal energy.
After each cycle of the circulatory motion, the temperature of the
liquid product increased from 0.2 to 0.3 °C. The food temperature
10 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16
Fig. 1. The physical principle of HTD processing (www.tekmash.ca, 2014).
Fig. 2. Experimental pilot-scale apparatus TEK-1.
in the stream was measured with built-in thermocouples (Honey-
well, USA) with accuracy of 0.1 °C; pressure was measured with a
pressure gage P16T2-4-100 (Indumart, Canada) with accuracy of
10 kPa. Electrical energy, introduced into the system, was mea-
sured with a current sensor TA17-03 (Omega Engineering, USA)
with accuracy of 0.1A. All parameters were recorded continuously
with LabView8.5 through a data acquisition interface USB-6008
(National Instruments, USA).
2.2. HTD processing
Fully ripened blueberries (80 kg) were provided by PEI Berries
Ltd, Montague, PE, Canada. Initial moisture content was
86.5 ± 0.7%, sugar content 7.8 ± 0.2°Bx and pH = 3.31 ± 0.01. Berries
were manually cleaned from non-edible residues (leaves, branches
etc.) and loaded in the processor at room temperature of about
20 °C. HTD process included simultaneous crushing and heating.
Centrifugal pump facilitated crushing of berries, but fine size
reduction actually occurred in the cavitator. Most of the crushing
occurred during the first two minutes, but processing went on until
the temperature reached 95 °C. The pasteurized product was then
filled into 250 ml glass jars, tightened with caps, inverted and
cooled overnight. Three batches of berries of 5.5 kg per batch were
processed within one day. One jar from each batch was used as a
replicate for analytical measurements and shelf-life study.
2.3. Quality evaluation
Effect of HTD on food quality was evaluated in terms of
chemical, physical and microbiological characteristics of the
product before and after HTD processing.
2.3.1. Chemical
Total polyphenols were measured with spectrophotometer
reading absorbance at 760 nm using Folin–Ciocalteau reagent with
gallic acid (GAE) as a reference standard (Singleton, 1999). Antiox-
idant activity was measured with oxygen radical absorbance
capacity (ORAC) using fluorescent substances (6-carboxyfluores-
cein) as an indicator of the reaction (Prior et al., 2003). Anthocya-
nins were determined by a pH differential spectrophotometric
method (Guisti and Wrolstad, 2001) using a microplate reader
Spectra Max 190 (Molecular Devices, California, USA). Total mono-
meric anthocyanin concentration was calculated as cyanidin-
3-glucoside (C3G) using an extinction coefficient of 26,900. Percent
polymeric color (tannins) was determined by measuring absor-
bance after bleaching anthocyanins with 20% potassium metabi-
sulfite (Guisti and Wrolstad, 2001) and expressed as a percentage
of the total color absorbance.
2.3.2. Physical
Particle size was measured using Laser Diffraction particle size
analyzer LS13320MW (Beckman Coulter, IN, USA). Viscosity was
measured according to ASTM standard D6080 using Brookfield dig-
ital viscometer LVDV-E (Brookfield Engineering Laboratories, USA).
Sedimentation was assessed by measurements of product viscosity
on different levels after settling.
2.3.3. Microbiological
Microbial load was determined from Total Aerobic Plate Count
(TAPC) and Yeast/Mold Count (YMC) in CFU/g. The effect of
processing was calculated as a log reduction with respect to initial
 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16
microbial load in raw material. Sensitivity of the method was lim-
ited to 10 CFU/g.
2.4. Shelf life evaluation
Jars with HTD processed blueberry were marked (number of
batch, order of filling) immediately after processing and divided
into two groups. One group was stored at +4 °C (cold storage),
another was kept at room temperature 20 °C in the food labora-
tory. Anthocyanin degradation was determined repeatedly on
day 8, 30, 48, 122, 189, 285, 376 and 546.
2.5. Statistical analysis
The optimum settings of temperature and holding time for the
HTD technology to maximize log reduction of microbial load was
determined through response surface analysis of a Central Com-
posite Design (Montgomery, 2013). The effect of processing on
quality (chemical, physical, and microbiological) indicators was
determined using a one way analysis of variance (ANOVA). This
was followed by multiple means comparison using the Least
Significant Difference (LSD) method at 1% level of significance. A
1% level of significance was used to protect Type I experiment wise
error rate from over inflation due to the relatively large number of
means. The model assumptions (normality and constant variance
of the error terms) were verified by examining the residuals as
described in Montgomery (2013). The first order differential model
was used to describe kinetics of product temperature and kinetics
of anthocyanin degradation. The error term for the regression
model was also assumed to be independent with normal distribu-
tion and constant variance. The model parameters were estimated
iteratively, and the validity of the assumptions was verified by
examining the residuals (Bates and Watts, 2007).
3. Results and discussion
3.1. Thermodynamics of HTD processing
Hydrodynamic heating in the closed system restricts mass trans-
fer, but allows energy transfer; so, it could be considered as closed
system process. According to the first law of thermodynamics, all
energy, supplied into the closed system, is used for work and heat-
ing. Heating occurs solely due to the viscous dissipation (friction)
within the system. High turbulence increased the entropy of the
system, maximizing the heating rate. This process is irreversible.
Energy input into the system was quantified by measurements
of electric current consumed by the motor. The current depended
on the hydraulic resistance of the closed system and cavitation
mode. Cavitation efficiency depended on the gas/liquid (G/L) volu-
metric ratio and was evaluated from the pump power input.
Amount of gas in the closed system (dissolved in the water and
released from cells during crushing of biomaterial) significantly
affected power input. Power input decreased with the increase of
air in the system, dropping to 0.7 kW when G/L achieved 0.15.
Results of instantaneous measurements of power input, tempera-
ture and pressure in HTD batch are shown in Fig. 3.
Temperature increased asymptotically, reaching 95 °C in
45–47 min. First order kinetics of product temperature accounted
for heat dissipation from the metal surface of the food processor.
The fitted asymptotic regression model that describes the change
in temperature as a function of processing time (t is in minutes) was:
T ¼ 140  120e0:021t
The heating rate decreased with temperature from 2.5 at 20 °C
to 1.15 °C/min at 95 °C, which could be explained by increasing of
heat transfer with temperature. Due to thermal expansion of the
11
Fig. 3. Temperature (circles), pressure (squares) and electric power consumption
(triangles) in HTD batch processing.
liquid in closed system, the pressure inside of the tank increased
with temperature. It followed temperature, asymptotically reach-
ing 250 kPa at 95–100 °C. At this temperature pressure relieve
valve, adjusted to keep pressure below 250 kPa, released pressure
from the system. A slight decrease of power input with time was
observed, which could be related to the formation of air cavity
and/or decrease of product viscosity with temperature.
3.2. Efficiency of HTD energy conversion
In the closed system, energy is neither created nor destroyed; it
can only transform from one form to another. The overall HTD pro-
cess could be represented as a sequential conversion of electrical
energy into mechanical energy of rotating motor, then into kinetic
energy of moving liquid and finally into the cavitation energy,
which was used for both crushing and heating (Fig. 4).
Efficiency of energy conversion into heat was calculated from
energy balance. Power input into the system, calculated from cur-
rent measurements, was in the range of 1.75–1.95 kW. Considering
efficiency of AC electric motor in the range 0.92–0.95, the mechan-
ical energy on centrifugal pump was in the range (1.61–1.85) kW.
Considering efficiency of centrifugal pump in the range of 0.5–0.7,
only from 0.80 to 1.29 kW of supplied power was converted into
kinetic energy of moving liquid. As a result of multiple circling in
the closed loop, kinetic energy of viscous liquid was dissipated into
heat. Thermal energy, accumulated in the food stream, was calcu-
lated from the temperature measurements:
E ¼ c q V DT ð6Þ
where c is specific thermal capacity, (J/g K), q is the product density,
g/m3, V is volume, m3, DT is heating rate, °C/s.
Using experimental data of heating rate (Fig. 3), product ther-
mal capacity 4.18 J/g K and density 1.06  106 g/m3, internal heat
accumulation was calculated as 0.55–1.05 kW. Therefore, effi-
ciency of heating of liquid product was in the range of 0.69–0.81.
The rest of heat energy, generated in viscous dissipation, was used
for heating of equipment metal parts and heat transfer to environ-
ment. Energy efficiency of HTD apparatus for liquid heating could
be further improved with thermal insulation of heated surfaces.
It is important to mention that calculation was done without con-
sidering energy for crushing and homogenizing of raw material.
3.3. Effect of HTD processing on chemical characteristics
ð5Þ
The effect of HTD processing on physico-chemical characteris-
tics and nutritional value of wild blueberry was evaluated by
analytic measurements of the corresponding indicators before
12 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16

Fig. 4. Energy conversion in HTD food processor.

and after processing (Table 1). From Table 1, it can be seen that
HTD processing increased caloric value of the product, possibly
due to conversion of polysaccharides into monosaccharides.
Increased sugar content, determined by Brix and HPLC measure-
ments, on the background of dietary fiber decrease, supports this
conclusion. Analysis of fatty acids showed twofold increase of
monounsaturated and polyunsaturated fatty acids, which could
be due to the partial disintegration of seeds. Effect of HTD process-
ing on moisture content, pH, macro- and microelements was very
small.
The effect of HTD processing on bioactive compounds was esti-
mated by measuring antioxidant activity (ORAC), total phenolics,
anthocyanins and tannins (Fig. 5). Measurements were carried
out immediately after processing (HTD) and in 1, 2, 4 and 8 weeks
after processing. Fresh (F) and crashed (C) blueberries were used as
controls. The absence of significant difference between F and C for
all measured characteristics indicated that crashing of wild blue-
berries in oxygen-free environment did not affect amount of bioac-
tives, initially presented in fresh blueberries. Time series showed
positive correlation between total phenolics, ORAC and anthocya-
nins, while negative correlation with tannins, probably due to
the temperature-induced polymerization of monomeric phenolics.
Fig. 5A shows a 15% increase in antioxidant capacity of HTD-
processed as compared to fresh berries. Apparently, size reduction,
thermal treatment and cavitation facilitated the process of releas-
ing of bioactive compounds in solution, making them available for
analytical measurements and eventual consumption. These results
are in agreement with those of thermally-induced release of bioac-
tive components from fiber matrix (Parada and Aguilera, 2007).
From Fig. 5B we can see that amount of total phenolics in HTD-pro-
cessed pasteurized blueberry was comparable to fresh blueberry,
probably due to the low oxidation. The same high retention of
phenolics was observed during the eight weeks storage at cold
(+4 °C) and room (+20 °C) temperatures, which proved initial
hypothesis about positive effect of HTD processing on the retention
of bioactive phenolics.
Monomeric anthocyanins are known to be sensitive to thermal
or enzymatic degradation (Brownmiller et al., 2008). Results of our
study, presented in Fig. 5C showed that compared to fresh blueber-
ries, the amount of anthocyanins dropped by 10% in crushed and
by 25% in HTD-processed blueberry. It could be explained by dis-
ruption of cells, which created conditions for PPO oxidation (Lee
et al., 2002) and accelerated reactions of phenolic polymerization
(Skrede et al., 2000). The hypothesis about thermal inactivation
of PPO at 95 °C pasteurization was supported by higher retention
of monomeric anthocyanins during eight weeks storage (Fig. 5C).
The effect of temperature on anthocyanins retention in pasteurized
product during eight weeks after processing was not significant.
The increasing trend in the percent of tannins just after HTD
processing (Fig. 5D) on the background of decreased anthocyanins
reflected the fact of partial phenolic polymerization. Tannins are
by-products of phenolic oxidation, which in our study served as
an indicator of oxidative processes. However, disproportion
between initial tannin formation (65%) and anthocyanin degrada-
tion (25%) indicated that certain amount of monomeric anthocya-
nins (about 40%) was released from fiber matrix. Measurements of
tannins during eight weeks after processing (Fig. 5D) showed low
level of oxidation, which was almost independent of temperature.
We can conclude that HTD processing did not jeopardize the qual-
ity of the product. Even eight weeks after processing, retention of
bioactive phenolics in HTD-processed blueberry was still above
90%.

Table 1
Nutritional value of wild blueberry before and after HTD processing.

Nutrition indicators Component Before processing After processing Units

Caloric value FBDG subtracted 45 53 Cal/100 g
Moisture Vacuum oven (70 C/16 h) 85.8 87.0 %
°
Brix Refractometer 7.8 8.5 Bx
pH 3.31 3.39 pH
Carbohydrates Carbohydrates, total 13.2 12.2 %
Total dietary fiber 4.4 1.9 %
Insoluble fiber 3.0 0.3 %
Soluble fiber 1.4 1.6 %
Sugars by HPLC Total sugar 7.04 8.35 %
Fructose 3.71 4.41 %
Glucose 3.33 3.46 %
Sucrose 0.00 <0.03 %
Maltose 0.00 <0.04 %
Fatty acid analysis profile Total fatty acids 0.160 0.285 %
Saturated fatty acids 0.030 0.029 %
Monounsaturated fatty acids 0.020 0.054 %
Polyunsaturated fatty acids 0.090 0.183 %
Trans fatty acids 0.000 <0.001 %
Omega-3 0.000 0.068 %
Omega-6 0.000 0.116 %
Cholesterol by GC <1.00 <1.00 mg/100 g
Polyphenols Total by FC 368 370 mg GAE/100 g
 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16 13

Fig. 6. Particle size distribution in HTD-processed (A) and blended (B) blueberry.

geneous suspension, including partial crushing of seeds, which is

not possible with conventional blending. HTD resulted in more
uniform distribution of small particles with 50% of particles less
than 0.27 mm, while blended blueberry had median characteristic
size of 0.82 mm. On the low end, HTD provided fine crushing with
25% of particles smaller than 0.12 mm, while blended blueberry
contained only 5.6% of small particles. Bi-modal distribution with
two peaks at 150 lm and 600 lm was explained by co-existence
of suspended small particles and coarse fraction (partially crushed
seeds), which could be easily removed from the stream by filtering
with 400 lm sieve. For the industry fine crushing was the desirable
attribute because of more stable texture and better availability of
nutrients.

Fig. 5. Effect of HTD processing on blueberry bioactives: phenolics (A), antioxidants
(B), anthocyanins (C) and tannins (D). F – fresh berries, C – crushed berries. Cold
storage (+4 °C) is in blue, room temperature (+20 °C) is in red, striped. For each
characteristic, means (bars) sharing the same letter are not significantly different.
(For interpretation of the references to color in this figure legend, the reader is
referred to the web version of this article.)
3.4.2. Viscosity
Particle size distribution determined product viscosity, which is
an indicator of organoleptic properties and texture stability.
Viscosity measurements of HTD-processed blueberry at low shear
rates from 0.02 to 6.0 s1 showed non-Newtonian pseudoplastic
rheological behavior (Fig. 7). Relationship between viscosity g
and shear rate c was described with power-law rheological model
(Falcao et al., 2009):

g ¼ KðcÞn1 ð7Þ
3.4. Effect of HTD processing on physical characteristics

Physical characteristics of whole blueberries before processing

were determined by three structural components: skin (6–8% in
overall volume), seeds (1.5–2%) and parenchyma (90–94%) with
different texture. Because of high fiber content, skin is partially
digestible, while seeds are not digestible. The only digestible part
of the fruit is a parenchyma with average moisture content of
88–90%.
HTD processing converted whole blueberry into homogeneous
suspension of skin, parenchyma and partially crushed seeds.
Physical characteristics of blueberries after HTD processing were
determined by measuring particle size distribution, viscosity and
sedimentation in the liquid product.

3.4.1. Particle size

Particle size distribution of HTD-crushed wild blueberry as
compared to blended with Power Pro blender (Black and Dekker,
USA) is presented in Fig. 6. In both cases energy input per unit mass
was 48 kJ/kg and processing time was 2 min. Particle size analysis
proved that HTD provided better crushing of whole berry to homo-
Fig. 7. Rheological behavior of HTD-processed blueberry with increasing (blue) and
decreasing (red) of shear rate. Dots represent experimental points and lines
represent fitted power-law model. (For interpretation of the references to color in
this figure legend, the reader is referred to the web version of this article.)
14 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16

where K is consistency index, Pa sn, n is the flow behavior index

(dimensionless).
Fitting of coefficients K and n across the range of shear rates and
then comparison of the coefficients showed that difference
between descending and ascending parts of the curve are statisti-
cally significant. The area of hysteresis represented energy lost in
the process of non-reversible viscous dissipation.
Effect of processing temperature on product viscosity was
significant. Measurements of viscosity showed 2.65 ± 0.11 Pa s for
samples, processed at 85 °C and 1.5 ± 0.038 Pa s for samples pro-
cessed at 95 °C. Consistent decreasing viscosity with temperature
could be related to thermal pectin degradation (Fraeye et al., 2007).

3.4.3. Sedimentation
Immediately after processing there was no product sedimenta-
tion in the jar. Effect of eight weeks storage on product sedimenta-
tion and general uniformity was estimated by measuring viscosity
of undisturbed product at the top, center and at the bottom of
250 ml glassy jar and fitting experimental data with the same
power-law model (Eq. (7)). Comparison of the model parameters
(K, n) for the three levels (top, center, and bottom) as well as the
two shear directions (increasing and decreasing) was conducted Fig. 8. Contour plot of log reduction as a function of temperature and holding time.
by fitting nested nonlinear regression models, and then testing
the significance of the incremental parameters by conducting extra
sum of squares analysis (Bates and Watts, 2007). Statistical analy- product lost 45.1% of anthocyanins. Based on our results, we can
sis showed no difference between viscosity on the top, center and conclude that retention of anthocyanins in HTD puree was better
bottom level, which supported initial hypothesis of stable texture than that in conventionally processed berries. For example, after
and low sedimentation rate. Based on our measurements and anal- 6 months of storage at 25 °C, non-clarified and clarified blueberry
ysis, we can conclude that HTD processing of whole blueberries juices contained only 23% and 15% of the original berry anthocya-
results in uniform viscous suspension with stable texture. High vis- nin (Brownmiller et al., 2008).
cosity of HTD-processed blueberry prevented product sedimenta- Kinetics of anthocyanins degradation was expressed using the
tion. Results obtained in this study demonstrated the potential of first-order exponential model. The analysis of experimental data
HTD processing for producing food with desirable texture, varying showed that the rate of anthocyanins degradation during cold
from thick juice to viscous puree. storage is less than half of that stored at room temperature. The
reaction rate constant k was found to be 1.51  103 days1 at
3.5. Effect of HTD processing on microbiological characteristics 4 °C and 3.33  103 days1 at room temperature. Activation
energy of anthocyanins degradation was calculated from Arrhenius
Initial microbial load in raw wild blueberries was in the range equation:
(0.9–7.0) 104 CFU/g. With instrumental sensitivity of 10 CFU/g,
the upper limit of sensitivity in log reduction calculation was Ea ¼ R lnðk2 =k1 Þ  ðT 1  T 2 Þ=ðT 2  T 1 Þ ð8Þ
below 4.0. Our results showed that D-values for HTD process were
Calculated value of 25.8–33.4 kJ/mol is much lower than 40.8–
22 min at 82 °C, 3.5 min at 85 °C and 0.4 min at 88 °C. Alterna-
52.5 kJ/mol, reported in literature for berries anthocyanins
tively, D-values, determined for thermal treatment of the same
(Moldovan et al., 2012). Lower activation energy implies that the
microbial load were 235 min at 82 °C, 18.8 min at 85 °C and
anthocyanins in the HTD-processed blueberry are less sensitive
2.5 min at 88 °C. These D-values were used to calculate z-values.
to temperature degradation than in aqueous and ethanol extracts
Effect of temperature and holding time on the microbial load
(Moldovan et al., 2012). Fitted models of anthocyanins degradation
reduction obtained from response surface analysis was repre-
can be used to predict anthocyanin concentration at any tempera-
sented in form of contour plot (Fig. 8).
ture. For example, using Eq. (8) for calculation of shelf-life of the
Based on the results of microbiological tests, it was concluded
product at the temperature 0 °C showed that reaction rate constant
that HTD processing of blueberries at 95 °C with the holding time
ko = 1.28  103 days1. Hence, half-life of anthocyanins at this
9 min provided the best quality of the blueberry product in terms
temperature is 540 days or 1.5 years. It means that HTD processing
of food safety. In order to determine the product stability and qual-
has significant potential to extend shelf-life without compromising
ity over a prolonged storage period, shelf life evaluation study was
quality. Results obtained in this study demonstrated potential of
carried out.
HTD processing for industrial manufacturing of innovative natural
whole foods with high nutritional and nutraceutical values.
3.6. Effect of HTD on product shelf life

Shelf life evaluation was based on the study of anthocyanin
degradation during 18 months of storage under room (20 °C) and
cold (4 °C) temperature. Both storage temperature and time signifi-
cantly affected the levels of anthocyanins in the blueberry puree
(Fig. 9).
Statistical analysis showed that 2 months of cold storage did
not affect retention of anthocyanins in HTD product. Cold storage
up to 6 months resulted in small losses (18.4%). As it was expected,
room temperature accelerated degradation rate: in 6 months
3.7. The benefits of HTD processing for food industry
Capital cost, energy requirements and food safety are the most
critical considerations for industrial acceptance of any novel
technology (Banholzer and Jones, 2013). Another consideration is
food texture, in particular highly viscous products, which narrows
the choice of technology. Our research showed that HTD could be
an excellent alternative to conventional technologies for pasteuri-
zation of viscous foods. Hence, we made an attempt to summarize
 A. Martynenko et al. / Journal of Food Engineering 152 (2015) 8–16 15

Fig. 9. Kinetics of anthocyanins degradation during storage (calculated per FW).

Table 2
Cost, energy requirements and food safety of viscous food pasteurizers.

Technology Capital cost of Energy requirements, Associated cost of Food safety risk Source
equipment MJ/m3 production, $/m3
Tubular pasteurizer (conventional) >$50–75,000 360–540 $10–15 Low Sampedro et al. (2013)
HTDT $15,000 300–430 $8–12 Low www.tekmash.ca
HPP high temperature (90 °C) $1–3 Million 13,350 $371.65 Low Buckow (2012)
HPP low temperature (5 °C) $1–3 Million 5000 $138.07 Medium Buckow (2012)
PEF $0.8–1 Million 1000–2500 $30–70 Does not work on spores Ramaswamy et al. (2011)
UV $15,000–$30,000 700–1000 $20–30 Effective only on surface Garland and Donahue (1998)

all available information about pasteurizers of viscous foods. The
comparison is presented in Table 2.
It follows that most of novel technologies, like HPP, PEF or UV,
fall in the category of very expensive or high energy consumption.
Only one of them (HPP, high temperature) is acceptable from the
point of food safety requirements. Conventional and HTD technol-
ogy are the most competitive and attractive for industry with
respect to capital cost, energy requirements and food safety.
Additional benefit of HTD processing as compared to conventional
processing is product quality, which is difficult to evaluate at the
moment in dollar value.
4. Conclusions
Our study proved desirable characteristics of novel HTD pro-
cessing technology on the retention of bioactive phenolics, includ-
ing anthocyanins in heat-sensitive foods. Amount of bioactives in
HTD-processed pasteurized blueberry was comparable with that
of fresh blueberry, probably due to the low oxidation. Immediately
after HTD processing at 95 °C, the amount of total phenolics did not
change, ORAC increased by 15%, anthocyanins decreased by 25%
and tannins increased by 65%. Eight weeks after processing, the
retention of bioactive phenolics was above 90%.
HTD provided fine crushing of fresh blueberry, including partial
crushing of seeds, which is not possible with conventional blend-
ing. Viscosity of HTD-processed blueberry was in the range 1.45–
2.65 Pa s, which prevented product sedimentation.
Shelf life study of HTD-processed blueberry showed exponential
kinetics of anthocyanins degradation with activation energy in the
range 25.8–33.4 kJ/mol. Long-term retention of anthocyanins in
HTD food was better than that in conventionally processed products.
Acknowledgements
Authors would like to thank Kevin Carver (PEI Berries Ltd.) for
providing blueberries and support for this research. This research
was also supported by NSERC – Canada Discovery Grant RGPIN
355740-08 and NSDA Technology Development Grant DEV27-65
to Dr. Alex Martynenko.
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