Journal of Food Engineering 124 (2014) 43–53

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Journal of Food Engineering

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

Effect of particle size and temperature on rheological, thermal,

and structural properties of pumpkin flour dispersion
Jasim Ahmed a,⇑, Muhammad Al-Foudari a, Fatimah Al-Salman a, Abdulwahab S. Almusallam b
a
Food and Nutrition Program, Kuwait Institute for Scientific Research, P.O. Box 24885, Safat 13109, Kuwait
b
Chemical Engineering Department, Kuwait University, Kuwait

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

Article history: Controlling the rheological properties of dispersion has been of great interest in the food processing
Received 24 March 2013 industry. Effects of particle size and temperature on oscillatory rheology of pumpkin flour dispersion
Received in revised form 25 September 2013 were studied. Fresh pumpkin was freeze-dried, grinded and sieved through selected screens to obtain
Accepted 26 September 2013
desired particle size fractions (74–841 lm). Most of the particles are spherical in shape. The glass
Available online 4 October 2013
transition temperature (Tg) and the melting temperature (Tm) of starch–lipid complex varied with particle
size which is believed to be due to compositional variations. Rheological measurement of reconstituted
Keywords:
particles as a function of temperature (10–90 °C) and concentration (4–10% w/w) indicated a solid-like
Particle size
Mechanical strength
behavior (G0 > G00 ). Sediment volume fraction (/) of isolated particle dispersions indicated a gradual
Glass transition temperature decrease with decrease in particle size, which directly influences the mechanical strength and visco-elas-
Viscoelasticity ticity of the dispersion. Particle size influenced the mechanical rigidity of pumpkin dispersion markedly
Sediment volume fraction whereas the temperature had the least effect. An unexpected increase in G0 of finest particle containing
Complex viscosity dispersion with temperature could be associated with gelatinization of starch and flocculation of particles
with broken cell walls. Microscopic observation revealed the presence of a continuous network for the
finest particle dispersion, as opposed to discontinuous one for other particle sizes.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction
Pumpkins belong to the family Cucurbitaceae and the genus
Cucurbita. Pumpkins and squash are available in different shapes
and sizes with attractive orange colors around the world. It is a
good source of carotenoids with the presence of relatively high
contents of provitamin A carotenoids (principally b-carotene, a-
carotene, and sometimes b-cryptoxanthin) (Speek et al., 1988;
González et al., 2001). Furthermore, pumpkins contain several
biologically active components including polysaccharides, proteins
and peptides, para-aminobenzoic acid, phenolic compounds and
terpenoids and sterols (Kuhlmann et al., 1999). It is mostly
considered to have active hypoglycaemic properties and it is
reported that fruit pulp has anti-diabetic effects (Adams et al.,
2011). Pumpkin flour powder (PFP) with or without sugar showed
a significant increase in plasma insulin and reduction in blood
glucose (Ju and Chang, 2001). Pumpkin mesocarp tissue has been
used as a food matrix for iron supplement, and it is considered as
a promising raw material for functional food product development
(de Escalada Pla et al., 2009).
⇑ Corresponding author. Tel.: +965 24989789.
E-mail addresses: jahmed2k@yahoo.com, jaahmed@kisr.edu.kw (J. Ahmed).
Pumpkin is used in various forms (e.g. puree, dry slice, powder)
which are commonly used as an ingredient in pies, soups, sauces,
stews, breads, instant noodle, and many other preparations as well
as a natural coloring agent in pasta and flour mixes. Pumpkin
shows a great diversity of texture in the cooked form, ranging from
the smooth, pasty, dry, high-starch buttercup types to the stringy,
watery, wet, low-starch types (Corrigan et al., 2001). It is difficult
to understand whether texture attributes are inherited or
attributed to constituents.
Size reduction is an important unit operation where the ratio of
surface area to volume of a food material is increased. Size reduc-
tion results in a mixture of particles, ranging a broad distribution
starting from a larger size to a fine particle whereas sieving sepa-
rates milled flours on the basis of particle size. The fullest descrip-
tion of a powder is given by its particle-size distribution (Snow
et al., 1999). Because of the wide variation in the size and shapes
of the particles and related properties in suspensions, it is really
difficult to understand the contributing factors that affect the rhe-
ology. It is now accepted that the food powder properties are
strongly dependent on the chemical composition and the surface
properties of the particles (Cuq and Rondet, 2011). Separation of
particles in uniform size range could provide uniform functional
properties. Furthermore, the interaction of those known particle
sizes with other ingredients could provide better understanding

0260-8774/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.jfoodeng.2013.09.030
44 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53
Nomenclature
List of abbreviations
ASTM American Society for Testing and Materials
ANOVA Analysis of variance
DSC Differential scanning calorimetry
LVR Linear visco-elastic range
AOAC Official Methods of Analysis
PF Pumpkin flour
PFD Pumpkin flour dispersion
PFP Pumpkin flour powder
RSM Response surface methodology
SEM Scanning electron microscope
List of symbols
x angular frequency, Hz
P bulk density, kg/m3
g* complex viscosity, Pa s
A constant
G0 elastic modulus, Pa
of food structure and stability during food formulation, quality
control and product development.
Limited reports are available on the particle size dependency on
rheological properties of food materials. Kerr et al. (2001) reported
significant effects of particle size on the functionality of cowpea
flour and reported textural problem with finer particles. Hayashi
et al. (1976) obtained a good bread volume using fine fractions of
hard red spring wheat flour, whereas coarse fractions were recom-
mended for the cake applications. The viscoelastic behavior of sus-
pensions has also been assessed by particle size distribution and
shape as well as the volume fraction of particles (Nakajima and
Harrell, 2001; Servais et al., 2002) and the particle–particle interac-
tions (Shah et al., 2003). However, no attempt has been made to
study the effect of specified particle range on the food rheology
although it has tremendous effect on the food dispersion and even
quality control of food suspensions especially soups and beverages.
The specific particle size range and the volume fraction of swol-
len particles significantly influence the rheology of pumpkin flour
dispersion (PFD). The objectives of this research work were to
determine the effects of particle size, temperature, concentration,
and their interactions (temperature–particle size) on rheological
behavior of pumpkin flour (PF) particles dispersion.
2. Materials and methods
2.1. Sample preparation
A single batch of mature fresh pumpkin (Cucurbita moschata)
samples was purchased from the local market in the state of
Kuwait during the winter season of 2012–2013. Samples were
washed thoroughly, peeled and cut into small pieces with a sharp
knife followed by manual separation of seeds from the pulp; finally
pulps were macerated into puree and freeze dried. One set of fresh
pureed sample was collected before freeze drying for rheological
measurement. For the freeze drying operation, the samples were
frozen in a freezer, and later transferred to the freeze-drier (GAM-
MA 2-16 LSC; Martin Christ GmbH, Osterode am Harz, Germany)
for 38 h at a temperature between 47 °C and 50 °C, and a pres-
sure of 0.7 Pa. Dried PF samples were grinded in a laboratory size
grinder (Robot Coupe R5, France), and passed through a series of
U.S. Standard sieve numbers 20, 30, 50, 100 200 and 230 mesh
n frequency exponent
Tg glass transition temperature, °C
HS height of the sediment, m
S particle size, lm
g00 imaginary part of complex viscosity
Xi and Xj independent variables
b0, b1; bii; bij response surface coefficients
Y measured response in RSM
e random experimental error
g0 real part of complex viscosity
/ sediment volume fraction
Tm starch–lipid melting temperature, °C
HT total height of the dispersed sample, m
L tristimulus color value, lightness
a tristimulus color value, redness
b tristimulus color value, yellowness
G00 viscous modulus, Pa
(Endecotts, London, UK), manually. The fractions obtained from
those sieve analysis retained by the sieve were designated as 841
(20; +30), 595 (30; +50), 297 (50; +100), 149 (100; +200),
and 74 (200; +230) lm. The ve sign represents pumpkin flour
particles passed through the sieve and the retained particles are
expressed through +ve sign. Fractionated samples were packed in
amber glass bottles and stored at 5 °C till further use.
2.2. Physico-chemical properties
The proximate compositions of the ground PF samples were
analyzed according to AOAC methods (AOAC, 2002) for the deter-
mination of moisture, ash, and crude fat contents. Protein was cal-
culated as nitrogen content (N)  5.3. Protein for each particle
fraction was estimated by the CHNS analysis based on combustion
method (AOAC, 2002). Total soluble solids and pH were measured
by a refractrometer (Atago CM-780N-Plus; Bellevue, WA, U.S.A.)
and pH-meter (Sension 3, Haach Co, Loveland, Columbia, USA),
respectively. The loose bulk density was determined by weighing
the mass of the dried powder sample which freely was poured in
a 100 ml graduated cylinder and expressed as weight per unit vol-
ume (kg/m3) (ASTM D7481-09). The volume of bulk aggregate
material includes the volume of the individual particles and the
volume of the voids between the particles.
2.3. Determination of sediment volume fraction
The volume fraction of the PFD of different particle sizes was
measured using a simple centrifugation method as described by
Hemar et al. (2011) for carrot cell wall particles dispersion with
some modification. Simply, 1 g of flour was dispersed in 20 ml
deionized water in a graduated centrifuge tube, mixed well in a
vortex and kept for 6 h for hydration followed by centrifugation
(Beckman GS-6R, USA) at constant centrifugation force (3000g) for
60 min.
After centrifugation, the total height HT of the sample and the
height of the sediment HS were measured and the effective volume
fraction / occupied by the PF particles was expressed as:
HS
/¼  100 ð1Þ
HT
 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53
Eq. (1) is valid only for closely packed particles without interstitial
space and without damage during the packing. The volume fraction
determination was performed at least in duplicate.
2.4. Tristimulus color measurement
Visual color was measured using a Hunter colorimeter model
ColorFlex (Hunter Associates Laboratory, Reston, VA) in terms of
L (lightness), a (redness and greenness) and b (yellowness and
blueness) as described earlier by Ahmed et al. (2002) for green lea-
fy vegetables. The instrument (45°/0° geometry, 10° observer) was
calibrated with a standard black and white tile followed by mea-
surement of samples. A glass cell containing the PFD was placed
above the light source and L, a and b values were recorded. Color
measurements were taken in triplicates, and average values were
taken for calculation.
2.5. Rheological measurement
Oscillatory rheological measurements of fresh ground sample and
PFD were carried out using a Discovery Hybrid Rheometer HR-3 (TA
Instruments, New Castle, DE, USA). Samples were placed in a 1000-
lm gap between two stainless steel parallel plates (plate diameter
40 mm). The sample perimeter was covered with a thin layer of
high-temperature-resistant silicone oil to prevent sample dehydra-
tion. The sample temperature was controlled by a peltier system
and monitored by platinum resistance thermometer sensors (accu-
racy of ±0.1 °C) which are positioned at the upper and lower plates.
The studied temperature range for oscillatory measurement was
10–90 °C. A sample concentration of 10% (w/w-10 g flour in 90 ml
water) was used throughout the work for rheological study except
for concentration effect where a range of 4–10% (w/w) was used.
Small-amplitude oscillatory strain sweep experiments (0.001–
10%) were performed, and the elastic (G0 ) and viscous (G00 ) shear
moduli, at a constant frequency of 0.1 Hz were monitored to deter-
mine the limit of the linear visco-elastic region (LVR). The LVR was
carried out for the entire studied temperature range (data are not
shown), and the measurement was carried out accordingly. Fre-
quency sweep tests (0.01–10 Hz) were carried out in the linear re-
gime, at constant strain (0.03) at selected temperatures. Following
an initial equilibration of samples for 5 min at 10 °C, ramp heating
was carried out at 5 °C/min to an endpoint of 95 °C (non-isother-
mal heating) at a frequency of 1 Hz. All rheological measurements
were carried out in triplicate and rheological parameters were ob-
tained directly from the manufacturer supplied computer software
(TRIOS, TA Instruments, New Castle, DE, USA).
2.6. Differential scanning calorimetric (DSC) measurement
A differential scanning calorimeter (DSC) (TA Q 2000, TA Instru-
ments, New Castle, DE, USA) was employed to measure the thermal
analysis for PF and dispersions. The DSC was calibrated with indium
and sapphire for temperature and heat capacity calibration. The
samples (10–12 mg) were run at a 10 °C/min heating/cooling ramp
in heating–cooling cycles in a nitrogen atmosphere (flow rate 50 ml/
min). The samples were heated from 20 to 180 °C to detect ther-
mal properties including, glass transition temperature (Tg), gelatini-
zation of starch and starch–lipid complex in dry fraction and in
dispersion. An empty pan was used as a reference. The DSC
measurements were done in triplicate. Thermal transitions of PFD
were measured for the peak gelatinization (Tm) and the melting
temperature (Tm) of starch–lipid complex. Instrument software pro-
vides the onset temperature, end point temperature, and the change
of heat flow of the glass transition region. The glass-transition mid-
point value was calculated as the average of the onset and end point
values and reported as the glass transition temperature.
45
The enthalpy (DH) of the transition (associated with starch–li-
pid complex) was calculated from the area of the peak endotherm
using the Universal Analysis Software (version 4.5A, TA Instru-
ments, New Castle, DE, USA).
2.7. SEM and microscopic observation for average particle size and
tissue structure
The microstructure and particle dimension of PF particles were
examined through a scanning electron microscope (SEM) (JEOL,
JSM-5410LV, Tokyo, Japan). Each sample was coated with gold in
a sputter coater (Structure Probe, West Chester, PA) before being
scanned and photographed at 100 and 250 magnification. Par-
ticle size was measured by the software attached to the instrument
which allows for detailed (average particle diameter and
maximum length) measurements. About 50 particles were chosen
randomly for the particle size measurement. A new generation
DMRX Polarizing Microscope fitted with Image Processing
Software (QWIN, Leica, Germany) was also used for particle size
measurement and to study the heated PFD tissue structure.
Microscopy of particles was carried out under crossed polarized
Nicols using 5 and 10 objectives.
2.8. Experimental design and statistical analysis
Since response surface methodology (RSM) designs have many
advantages like adequate distribution of information across the
experimental range (rotatability), good lack of fit detection, the fit-
ted values are very close to the observed ones and they require the
minimum number of treatment combinations (Kokkinidou and
Peterson, 2013), and therefore, RSM has been selected to study
the simultaneous effect of temperature and mesh size on rheolog-
ical characteristics of PFD at a constant concentration of 10%. The
experiments were based on a central composite rotatable design.
Five levels of temperature (10, 30, 50, 70 and 90 °C) and particle
size (74, 149, 297, 595 and 841 lm) were selected. The total num-
ber of experiments was 13 with five replications of the center
point, as shown in Table 1. The independent variables temperature
and mesh size were selected to optimize the responses g* and G0 at
1 Hz.
A general second order model is mostly used in response
surface methodology for predicting individual Y variables (Khuri
and Mukhopadhyay, 2010). The model proposed for each response
of Y is:
X
k XX X
k
y ¼ b0 þ bi xi þ bij xi xj þ bii x2ii þ e ð2Þ
i¼1 i <j i¼1
where Y is the measured response associated with each factor level
combination, b0 is the intercept, b1; bii; and bij are linear, quadratic
and interaction coefficients of the model, Xi and Xj are the indepen-
dent variables in coded values, and e is a random experimental error
assumed to have a zero mean. The regression analysis, analysis of
variance (ANOVA) of data was carried out using the Minitab Statis-
tical Software (Version 16; Minitab Corp., USA) to fit second order
polynomial equations for all response variables. Lack-of-fit tests
were performed on the fitted models. For statistical tests, signifi-
cance was defined at P 6 0.05.
3. Results and discussion
3.1. Proximate composition
Freeze drying of pumpkin pulp into flour significantly reduced
the moisture content to 6.7% (wet basis). The ash content and
crude fiber of the flour were 5.6% and 11.7%, respectively in wet
46 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53

Table 1 However, a sudden drop of bulk density to 562 kg/m3 was recorded
Level of independent and response variables in experimental design. for particle size of 74 lm. Similar decrease in bulk density with
Treatment Independent variables Response particle size has been reported earlier for sweet potato powder
variables (Grabowski et al., 2006). The decrease has been explained by con-
X1 X2 Temperature Particle size G0 (Pa) g* sidering the stickiness of particles during dehydration and also
(°C) (lm) (Pa s) from product agglomeration (Goula et al., 2004). Although particles
1 0 1.41 50 841 47,458 7650 may be small when measured individually, these agglomerates
2 0 0 50 297 16,695 2672 take up a larger volume and, thus, would contribute to a smaller
3 1 1 70 149 10,093 1611 bulk density.
4 1.41 0 90 297 15,599 2500
5 1.41 0 10 297 19,249 3089
6 0 0 50 297 16,700 2673 3.4. Sediment volume fraction of dispersion
7 0 0 50 297 16,767 2675
8 0 1.41 50 74 96 16 The volume fraction (/) of suspended particles in aqueous dis-
9 1 1 30 149 9934 1501
persions of PF at 30 and 70 °C is presented in Fig. 2. Standard devi-
10 0 0 50 297 16,700 2670
11 1 1 30 595 40,801 6568
ations are not indicated for the results where estimations were
12 1 1 70 595 40,786 6297 made using mean values of two runs. The volume fraction repre-
13 0 0 50 297 16,790 2677 sents the particles occupancy after centrifugation and it mostly
estimates the effective volume fraction of the particles. PFD con-
taining particle sizes of 841 lm exhibited the highest / whereas
basis. The lipid and protein content of the flour was 1.04% and 9.1%, the least value was obtained for powder particles of 74 lm. Gener-
respectively. These values are relatively different from reported ally, it is expected that the magnitude of / increases with fineness
values for PF (Aziah and Komathi, 2009; See et al., 2007). The of the particle size. However, the opposite trend was observed for
difference is believed to be attributed to variations in geographical PF. The unusual trend could be attributed to cellular structure of PF
location, cultivar and method of sample preparation. The total and its water holding capacity. It is observed that more water was
soluble solids content and the pH of the pumpkin puree before absorbed by porous particles compared to finer particles. This is
freeze drying were 10.1 ± 0.2 °Brix and 6.31 ± 0.02, respectively. further evidenced from the microscopic study as discussed later.
It is worth to mention that particle fractions did not show any The largest hydrated particle is expanded almost two times (i.e. 8
significant difference in proximate compositions except nitrogen times volume increase based on spherical uniform particle) com-
content which is discussed later on. pared to 1.5 times (volume increase 3.4 times) for smaller one
(Fig. 4). Secondly, the PF particles were disrupted during shearing
and the cell walls separated from the endosperms especially for fi-
3.2. PF sieve analysis
ner particles (evident from microscopic study-discussed later on)
which is probably the cause for lower / value of 74 lm powder.
Particle mass (%) of ground PF after size distribution is shown in
Raising the temperature to 70 °C and heating isothermally for
Fig. 1. It was observed that the maximum weight percent of parti-
30 min causes no significant change in the / value except for the
cles (30%) were about 297 lm followed by 149 lm (29%), and
sample of particle size 74 lm. It clearly indicates that the coarse
74 lm (25%). The grinding process produced minimum weight
granules already absorbed the maximum amount of water. Similar
percent of coarser particles; about 1% and 15% of particles were
observation (constant granule sizes after heating) was made by
in the sizes of 841 and 595 lm, respectively. Overall, ground PF
Paterson et al. (2001) while working on corn starch from different
had a broader distribution of particle sizes.
sources.

3.3. Bulk density 3.5. PF particle size analysis by microscope and SEM

Particle size has a significant impact on bulk density. Generally, The particle sizes of the PF passed through sieves were observed
as particle size decreases the bulk density increases. Following this through microscope and SEM, respectively. The average particle
rule, the bulk density of PF powder increased linearly from 522 to size, the largest and smallest particle sizes are reported in Table 2.
756 kg/m3 when the particle size decreased from 841 to 149 lm. The finest fraction seemed to have smaller particle size by almost

40

30
% Particle mass

80
Volume fraction %

20 30C
60
70C
40
10
20

0 0
841 841
595
595
297
297
Particle size 149 Particle size 149
74 74

Fig. 1. Mass distribution of freeze dried PF powder particles after sieving. Fig. 2. Effect of particle size on sediment volume fraction of 5% (w/w) PFD.
 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53 47

20 times lower than the coarsest fraction. SEM and microscopic

images (Figs. 3 and 4) confirmed that the PF particles are irregular
in shape, and most of them are ‘spherical’ shaped. A mixture of
spherical, polyhedral and irregular shaped PF particles with less
smooth granule surfaces have been reported (Saeleaw and
Schleining, 2011). The larger particles were relatively more porous
than finer particles. The hydrated particles indicated the water
absorption capability of dried particles and the size of the particles
increased thereafter.

3.6. Color of particle fractions

The observed color values for PF with different particle sizes are
shown in Table 3 and the values are comparable as reported by
Kim et al. (2012) for orange color PF. Generally, the increase in
the particle specific surface area by comminution caused better
and more intense color values. As can be seen, decreasing the par-
ticle size caused an increase in the redness (+a value), yellowness
(+b value) and lightness (L value) values of PF. The color values L
and b decreased abnormally for 74 lm powder whereas +a value
decreased for 149 lm sample. Mostly, the attractive orange/yellow
color of PF is attributed by presence of lutein and b-carotene (Kim
et al., 2012). The drop in color values for finer particles could be
associated with removal of either lutein or b-carotene during size
reduction or disruption of tissue structure during high shear and
impact.

3.7. Thermal properties of particle fractions

Pumpkin flour can exist in different solid-state forms like crys-

talline, amorphous or both. Many food powders and food ingredi-
ent mixes have components mainly in the amorphous state. Starch
is semi-crystalline in nature and it shows both glass transition
temperature (Tg) and the crystalline melting temperature (Tm).
The glass transition temperature (onset, end and inflection) as
influenced by particle size reduction is presented in Table 4. The
coarser particles (841 lm) showed the minimum inflection Tg at Fig. 3. Scanning electron microscopy of pumpkin flour particles: (a) passed through
about 7 °C, and the finest particles (74 lm) possessed the highest 841 lm and (b) passed through 149 lm.
value of inflection Tg at about 13 °C although the change in Tg val-
ues were not systematic with particle size. The Tg is a very strong
particles (<15 lm) and starch was concentrated in fractions with
function of powder water content. As water is a plasticizer which
coarser particle sizes (>15 lm) (Wu et al., 1994). Vasanthan and
enhances molecular mobility, increased water content will lead
Bhatty (1995) studied scanning electron micrographs (SEM) of
to a reduction in the glass transition temperature. However, the
the coarse and fine barley fractions after an air classification and
moisture content of the studied sample was almost alike
reported that most of the small starch granules were concentrated
(10.16 ± 0.12). The onset Tg represents the demarcation above
into finer fraction. Furthermore, coarser particles had lower protein
which the molecules start to gain mobility or flow which will en-
and higher starch, and finer particles had higher protein and lower
able them to crystallize over time. The difference in observed Tg
starch. Based on those above information, it could be assumed that
with particle size must be attributed to the constituents (starch
both protein rich fraction and smaller starch granules contribute to
and proteins) of the particles itself. However, it is really difficult
the increase in Tg. The protein enrichment of fine particles is fur-
to claim the actual contribution of each major constituent (starch
ther supported by CHNS analysis data. The nitrogen (N) and carbon
or protein) to the particle here as the ground samples were not
(C) contents showed a difference in the magnitude of each fraction
separated by air classification which is mostly used in cereal
of particles. For example, the N and C-contents of coarser particle
starch/protein separation. It has been reported that the protein
(841 lm) fractions were 1.28 and 39.2 which changed to 1.42
after air classification was concentrated in fraction with fine
and 38.1, respectively for fine particle (74 lm) fraction.
DSC thermograms of PF with different particle sizes show an
Table 2 additional thermal transition peak in the temperature range of
Particle size analysis through SEM measurement of PF passed through selected sieves. 144–158 °C. These melting peaks are different from starch gelatini-
Sieve size (lm) Avg. particle Largest particle Smallest particle zation peak and it is believed that these endothermic peaks (Tm)
size (lm) size (lm) size (lm) are attributed to the melting of a complex between native lipids
841(20-mesh) 920 ± 38 1110 771 and starch/amylose (Bhatnagar and Hanna, 1994). Furthermore, it
595 (30-mesh) 414 ± 26 589 301 is reported in the literature that two types of complex formation
297 (50-mesh) 235 ± 21 333 136 (Type I and II) have been identified through DSC measurement;
149 (100-mesh) 122 ± 13 159 47 one at lower temperature range (96–100 °C) and another at higher
74 (200-mesh) 46 ± 06 71 12
temperature range (100–125 °C) (Biliaderis and Galloway, 1989;
*
Values (mean ± SD, n = 15). Biliaderis, 1992). The observed Tm values indicated that the
48 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53

157 °C to 144 °C (Table 3 and Fig. 5). The drop in Tm is noteworthy

especially when the particle size reduced to 149 lm or less. The
significant decrease in Tm for smaller particle fractions could be
attributed to the presence of small starch granules which melted
at relatively lower temperature than larger starch granules. The
necessity for heat to dissociate the complex between amylose
and its ligand suggests that there are certain forces that steady
the helix conformation (Putseys et al., 2010). The only processing
variable that had a significant effect on the formation of starch–li-
pid complexes was moisture. The Tm of the amylose–lipid complex
decreased significantly (119–124 °C) with multiple peaks occur-
ring when significant amount of water was added to the particles
to produce a 10% dispersion. It has been reported in the literature
that the semi-crystalline type IIa complexes melt around 115 °C
(Biliaderis et al., 1986). In literature, there are many evidences
where the presence of multiple peaks has been reported (Biliaderis
and Seneviratne, 1990; Bulpin et al., 1982). This multiplicity of
peaks could account for different kinds of lipids (Bulpin et al.,
1982; Raphaedelis and Papavergou, 1991), which could form com-
plexes with different structures (Raphaelides and Karkalas, 1988).

3.8. Rheology of PFD

The oscillatory measurements of all the samples were measured

by performing frequency sweeps in the linear viscoelastic region.
Fig. 6 illustrates representative rheological behavior of fresh pump-
kin pulp (10% w/w dispersion) at 30 °C, showing elastic modulus
(G0 ), viscous modulus (G0 0 ), and phase angle (°) as function of fre-
quency. The dispersion shows a predominantly solid-like behavior,
as indicated by the dominance of the G0 over the G0 0 . For example,
the G0 value was almost six times higher than G00 at 1 Hz. Further-
more, G0 increases systematically within the studied frequency
Fig. 4. Microscopic view of PF particles: (a) particle passed through 74 lm screen
and measured at 25 °C; (b) particle passed through 74 lm screen and measured
range (0.1–10 Hz). However, the G00 dropped at the similar condi-
after heat treatment; (c) particle passed through 841 lm screen and measured at tion except at higher frequency range. The G0 –x produces a
25 °C; (d) particle passed through 841 lm screen and measured after heat smoother curve with better reproducibility than G00 , which is prob-
treatment; (e) heated 149 lm; and (f) heated particles network passed through ably due to the more solid characteristic of the suspensions. Similar
74 lm.
observation has been reported for tomato suspension (Bayod and
Tornberg, 2011). The phase angle (°) decreased from 17 to 8.5 with
Table 3 the frequency indicating a gradual increase in solid-like property
Effect of particle size on tristimulus color values of pumpkin flour. which levelled off later on.
Particle size (lm) L value +a value +b value
3.9. Effect of concentration
841 65.13 ± 2.10 15.02 ± 0.73 28. 72 ± 1.43
595 65.18 ± 1.80 15.24 ± 0.92 31.24 ± 0.94
297 65. 70 ± 1.85 16.86 ± 1.10 34.17 ± 1.10
The mechanical rigidity of the heated PFD increased as the con-
149 73.22 ± 2.31 15.88 ± 0.83 37.43 ± 1.31 centration was increased from 4% to 10% (w/w). It is worth men-
74 68.43 ± 2.05 12.42 ± 0.65 32.35 ± 1.00 tioning that the mechanical strength was not detected below 4%
*
Values (mean ± SD, n = 3).
concentration of PF since the concentration is too low for rheolog-
ical measurement using parallel plate geometry. Therefore, 4% con-
centration can be considered as the minimum concentration to
Table 4 obtain a meaningful rheological structure/data. The G0 increased
Glass transition temperature and melting of starch–lipid complex of PF as function of abruptly (almost one log cycle) when the concentration was in-
particle size. creased further from 4% to 6%; above 6%, the value of G0 almost
Particle Tg (°C) Tm (°C) DHm (J/g) doubled. Such increment of the G0 of PFD as function of concentra-
size tion can be explained by the sediment volume fraction (/) of dis-
Onset Inflection End
persions which is found to be a direct function of concentration
841 1.40 ± 0.32 6.80 ± 1.01 13.76 ± 1.02 157.1 ± 1.54 137.6 ± 1.5
(data not shown). As the volume fraction increases gradually, the
595 1.06 ± 0.23 4.04 ± 0.85 9.96 ± 0.84 150.5 ± 1.33 180.7 ± 1.1
297 7.00 ± 0.80 12.12 ± 1.12 18.64 ± 1.22 157.8 ± 0.96 129.9 ± 1.2 G0 gradually increases faster than the loss modulus which has been
149 6.24 ± 0.72 12.09 ± 0.92 16.24 ± 1.01 144.0 ± 1.14 173.1 ± 0.8 attributed to significant compression and interpenetration of the
74 7.49 ± 0.64 12.97 ± 1.10 18.31 ± 1.42 145.5 ± 1.23 133.6 ± 2.1 stabilizing polymeric layer. Similar observation has been reported
*
Values (mean ± SD, n = 3).
by Luckham and Ukeje (1999) for polystyrene latex dispersion.
The rigidity of PFD at lower concentration is controlled by the vol-
ume occupied by the swollen granules (termed as ‘dilute’ regime),
complex comes under type II. Type II is more crystalline and is be- and, to a lesser extent, by the soluble fraction. While concentration
lieved to have a lamellar-like organization of amylose complexes was increased significantly, powder granules cannot swell to their
(Biliaderis, 1992; Biliaderis and Galloway, 1989). The Tm of the equilibrium volume due to limited availability of water, and then,
starch–lipid complex dropped with decrease in particle size from the rheological characteristics contributed primarily by the particle
 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53 49

0.0
––––––– 74 micrometer
gates) without any processing effect. Comparing the G0 , the PF of
– – – – 841 micrometer uniform particle size distribution (841 lm) showed a relatively
––– ––– 149 micrometer
higher G0 than that of sample with non-uniform particles. Consider-
-0.2
ing only hydrodynamic interactions, addition of equal amounts of
water to the individual particle volumes produces different suspen-
Heat Flow (W/g)

-0.4
sion viscosities. More water is required to fill the space between the
particles in the uniform size distribution (occupies more space than
widely distributed particles). Thus, the suspension of uniform size
-0.6 particles has less liquid between the particles compared to the
suspension consisting of packed particles, and therefore, the
suspension of uniform particles has higher viscosity. Further, it
-0.8 156.18°C has been argued that increasing the polydispersity for a given solids
143.51°C
volume fraction would decrease a suspension viscosity, which is
144.27°C also supported by the ‘Farris effect’ (Ferguson and Kemblowski,
-1.0
100 120 140 160 180 1991). Such study infers that not only the particles mean diameter,
Temperature (°C) but also the particle distribution is an important factor influencing
the rheology of suspensions (Sato and Cunha, 2009).
Fig. 5. Effect of particle size on starch–lipid complex melting behavior. The effect of particle size on the visco-elastic behavior of 10%
PFD at 70 °C is presented in Fig. 8. It is clearly evident that the com-
plex viscosity (g*) decreased gradually as particle size reduced
100000 20
from 841 to 74 lm. Similar observation has been reported for jabo-
ticaba pulp where increasing particle size from 64 to 550 mm pro-
moted a rise in the viscosity from 0.06 to 0.40 Pa s (Sato and Cunha,
G' G'' 2009). Generally, it is expected that finer particle size produces
15
more surface area and contributes to the higher mechanical
G', G'' (Pa)

δ
strength. However, our results showed the opposite trend. It is as-
δ (o)

10000
sumed that the ground PF was less porous and would be unable to
imbibe as much water as the coarse flour which is duly supported
10
by decreasing trend of / with fineness of particles as discussed ear-
lier. A blend of two distinct particle sizes (100 and 200 mesh) pro-
duces intermediate g* value which is higher than that of 200 mesh
but lower than 100 mesh. This increase might be attributed to dif-
1000 5
0.1 1 10 ferent interactions between pumpkin constituents with different
Frequency (Hz) particle size distribution. The complex viscosity (g of 10% PFD
can be well described by a quadratic polynomial equation as a
Fig. 6. Typical rheograms for 10% PFD containing particles size of 841 lm at 30 °C.
function of particle size (S) in the prescribed size limit (74–
rigidity of the swollen granules. Another explanation for increasing 841 lm) at 70 °C.
mechanical rigidity with concentration is based on the fact that
g ¼ 0:0064S2 þ 15:638S  941:77 ðR2 ¼ 0:99Þ ð4Þ
particles replaced water and increasing amount of particles pro-
duced a low water activity environment which favored hydropho-
bic interactions between pectin chains, and therefore, increased 3.11. Effect of temperature
the strength of the network (Genovese et al., 2010).
The gel rigidity (G0 ) of 149 lm PFD as a function of concentra- Non-isothermal heating of 10% PF with 74 lm particle size at a
tion (C) at 70 °C can be well described by a quadratic polynomial frequency of 1 Hz is presented in Fig. 10. As can be seen from Fig. 9,
relationship (Eq. (3)) with a coefficient of determination (R2) of
0.99. The equation is valid only at and above 4% (w/w) of PF con-
1000000 1000000
centration. Earlier a linear relationship between C and G0 has been G' fresh nonuniform PS G' PF nonuniform PS
reported for wheat and maize starch at concentration range of 6– G' PF 841 micrometer CV fresh nonuniform PS
30% (Ring, 1985). CV PF nonuniform PS CV PF 841 micrometer
100000
G0 ¼ 15:885C 2 þ 11:978C  239:38 where C  4% ð3Þ
η* (Pa.s)
G' (Pa)

3.10. Effect of sieving and particle size 100000 10000

Sieving of PF produces different particle sizes. Particle size distri-

bution plays an important role in dispersion rheology and food for-
1000
mulation. A comparative rheological study between the
reconstituted samples (10% concentration dispersion with uniform
and non-uniform particle size) and the whole pulp (10 oBrix) with
non-uniform particle size is shown in Fig. 7. It was observed that 10000 100
the fresh pulp possessed higher mechanical strength when com- 0.1 1 10

pared to the systems reconstituted with particles with and without Frequency (Hz)
sieving. The higher G0 values of fresh sample have been attributed to Fig. 7. A comparison of rheological behavior between uniform and non-uniform
a higher value of / than that of reconstituted sample and also to the particle size in 10% fresh and powder PFD (CV stands for complex viscosity and PS
retention of the original structure (anisometric cells and aggre- stands for particle size).
50 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53

100000 1000 100

Elastic modulus
10000 Complex viscosity

1000
η* (Pa.s)

100

η∗ (Pa.s)
G' (Pa)
100 10
10 841 micrometer 595 micrometer
297 micrometer 140 micrometer
74 micrometer Blend of 149 & 74 micrometer
1
0.1 1 10
Frequency (Hz)

Fig. 8. Effect of particle size on complex viscosity of 10% PFD at 70 °C.

as heating proceeds, there is a sharp increase in G0 and g* associ- 10 1

0 20 40 60 80 100
ated to starch gelatinization especially above the starch gelatiniza-
o
tion temperature of 73 °C (as detected from DSC measurement). Temperature ( C)
However the developed gel was not a strong one. The gel strength Fig. 9. Non-isothermal heating of 10% PFD passed through 74 lm sieve at a heating
is not improved even after non-isothermal heating followed by rate of 5 °C/min.
cooling to 25 °C (setback region) which is contrary to most of
starch dispersions (data not shown). This could be the nature of
pumpkin starch under heating–cooling condition and also the 100000 100000
material inability to form a viscous paste or gel after cooking and G' 30C G' 50C
cooling. The observed gelatinization temperature is very similar G' 70C G' 90C
to the pasting temperature of unripe pumpkin (72 °C) however CV 30C CV 50C
the value is relatively lower than that of ripe pumpkin (80 °C) CV 70C CV 90C
10000
(Roura et al., 2007). Further authors advocated that the differences

η* (Pa.s)
with samples would indicate changes in samples chemical compo-
G' (Pa)

sition due to maturity that could produce different starch interac- 10000
tions with endogenous materials (sugars, lipids, pectin and so on)
that would affect their behavior. Isothermal heat treatment of 1000
10% for 149 and 74 lm particles containing PFD are illustrated in
Fig. 10. A contradictory result was observed for those samples. It
is evident from Fig. 10a that the temperature has insignificant ef-
fect on both G0 –x and g*–x curves of PFD. An increase in suspen-
sion rigidity was observed at 70 °C which was basically caused by 1000 100
0.1 1 10
swelling of starch granules and gelatinization. PFD made from
Frequency (Hz)
74 lm particles exhibited an unexpected behavior during isother-
mal heating (Fig. 10b). In fact, the mechanical rigidity of dispersion (a)
having 74 lm particles was about 200 times weaker than the sus-
pension containing particle size of 149 lm at 30 °C. As it is men- 1000 1000
tioned in the earlier section, small starch granules are
concentrated in fine particles fraction which is believed to lower
the gel rigidity of dispersion. Furthermore, breakdown of starch
and disruption of cellular structure during comminution could be
100
possible other reasons for lowering the gel rigidity of fine pow-
dered dispersion. Both G0 and g* increased as function of heating
η* (Pa)
G' (Pa)

temperature; the increase was substantial at and above 70 °C 100

which is mostly attributed by gelatinization of starch in the parti-
cle. Microscopic studies supported the hypothesis cited above; it 10
was observed through microscope that most of the 74 lm particles
were ruptured and cell walls were broken. Such hypothesis was G' 30C G' 50C G' 70C
also supported by the development of a continuous gel network G' 90C CV 30C CV 50C
(Fig. 4f) whereas other particles produced only discontinuous gel CV 70C CV 90C
10 1
at similar condition (Fig. 4e). 0.1 1 10
The frequency (x) dependence of gel rigidity (G0 ) can be de- Frequency (Hz)
scribed by the power-type relationship:
(b)
G0 ¼ Axn ð5Þ
Fig. 10. Effect of temperature on oscillatory rheology of PF sample passed through
(a) 149 lm and (b) 74 lm sieve (CV stands for complex viscosity).
After linearization; ln G0 ¼ ln A þ n ln x ð5aÞ
 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53 51

where A is a constant and n is the frequency exponent (slope) 50000

whose value lies between 0 and 1.
The slope and intercept are calculated from the linear regres-
sion of ln x vs ln G0 . Table 5 provides magnitudes of slopes, inter- 40000
cepts and the goodness of fitting (R2) for 10% PFDs having different
particle sizes at selected temperature. Experimental data were fit-
ted well with R2 values being always higher than 0.95. The inter- 30000

η'' (Pa.s)
cept, A, of a definite particle size did not show any trend as
function of temperature. It is evident from the table that tempera-
ture had a minimal effect on the solid-like properties as assessed 20000
by slope, n, of PFD except for the dispersion having particle size
841 micrometer 595 micrometer
of 74 lm where temperature played a significant role by changing
the mechanical rigidity. The liquid-like property of 74 lm particles 10000
297 micrometer 149 micrometer
dispersion remained predominant up to 70 °C followed by a drop at
90 °C. The intercept (A) trends with particle size follow the afore-
mentioned behavior for G0 and g*; they decrease from 841 lm to 0
0 5000 10000 15000 20000
74 lm. A blend (1–1 ratio) of two uniform particles (74 and η' (Pa.s)
149 lm) exhibited predominant solid-like property (slope 0.05–
0.09) which was significantly different from fine particle (74 lm) (a)
dispersion.
800

3.12. Effect of particle size and temperature

74 micrometer
Although it is well established that the temperature greatly 600

influences the rheological properties of food products, limited

η'' (Pa.s)
studies have been carried out on particle size effect on food rheol-
ogy. When a system is filled with anisotropic particles, the type 400
and degree of orientation of the particles can have a significant ef-
fect on the rheological behavior (Metzner, 1985). Yoo and Rao
(1994) reported that there is a significant effect of particle size 200
on the flow properties of tomato puree. Both magnitudes of consis-
tency index and apparent viscosity of samples containing finer par-
ticles (60 mesh sieve) were higher than those of 40 mesh sieve 0
0 75 150 225 300
sample. From a practical standpoint, it will be more informative
η' (Pa.s)
to describe the effects of temperature and particle size on rheolog-
ical characteristics by a combined model. In this study, g* and G0 at (b)
1 Hz were related to temperature and particle size of 10% PFD by a
multiple regression analysis. Fig. 11. Dispersion of selected pumpkin flour particles in aqueous solution at 90 °C.

The effects of treatment variables as linear, quadratic, or inter-

action coefficients on response variables were obtained by ANOVA.
The predictive models developed for g* and G0 of 10% PFD were
considered adequate they possessed no significant lack-of-fit and
had a satisfactory level of R2. The linear terms were significant
for both g* and G0 (P < 0.05), whereas square and interaction terms
were insignificant. The R2 values were greater than 0.96 for all the
cases. The fitted equations were obtained considering only signifi-
cant terms to predict g* and G0 as shown below:
g ¼ 14S  558
G0 ¼ 85S  1924
where S is the PF particle size in lm.
The above equations indicated that particle size has significant
effect on both complex viscosity and elastic modulus, respectively.
The coefficient of linear term of particle size indicated a gradual in-
crease of rheological parameters as influenced by particle size.
3.13. Pumpkin flour particle dispersion in solution
Adequacy of PF particles dispersion in aqueous suspensions can
ð6Þ be analyzed by the Cole–Cole plot of the rheological data which
represents the relationship between real and imaginary parts of
complex viscosity (Joshi et al., 2006; Ahmed et al., 2010a,b). A
ð7Þ
smooth, semicircular shape of the plotted curves represents good
compatibility, that is, phase homogeneity in the solution, and any
deviation from the shape indicates nonhomogenous dispersion or
immiscibility. The g0 , the real part and g00 , the imaginary part of

Table 5
Slope of Eq. (5) for dispersion made by different PF particle size as function of temperature (R2 is reported after n value in the bracket).

Particle size (lm) 10 °C 30 °C 50 °C 70 °C 90 °C

n n n n
n A (Pa s ) n A (Pa s ) n A (Pa s ) n A (Pa s ) n A (Pa sn)
841 0.12(0.98) 52,029 0.11(0.98) 45,960 0.12(0.96) 46,005 0.11(0.98) 45,961 0.10(0.97) 39,681
595 0.10(0.99) 45,073 0.10(0.99) 38,482 0.11(0.97) 37,971 0.10(0.99) 38,481 0.09(0.99) 33,776
297 0.08(0.99) 19,136 0.07(0.98) 17,073 0.09(0.97) 16,374 0.07(0.99) 17,070 0.06(0.99) 15,547
149 0.06(0.99) 10,297 0.06(0.98) 9976 0.07(0.98) 9238 0.06(0.99) 9986 0.04(0.98) 8988
74 0.17(0.99) 56 0.24(0.95) 282 0.30(0.95) 90 0.24(0.99) 285 0.16(0.99) 670
Blend 74 & 149 0.06(0.99) 978 0.07(0.96) 1126 0.08(0.97) 931 0.09(0.99) 1120 0.05(0.96) 1235
52 J. Ahmed et al. / Journal of Food Engineering 124 (2014) 43–53
Table 6
Regression equations describing PF properties as function of particle size (S).
Property Equation
a 2
Bulk density q ¼ 0:0004S þ 0:157S þ 635 (10)
Volume fractiona / ¼ 0:0001S2 þ 0:160S þ 11 (11)
Complex viscositya g ¼ 0:0002S2 þ 18:1S  2185 (12)
Glass transition (13)
T g ¼ 0:00002S2  0:025S þ 16
Starch–lipid melting point T m ¼ 0:00002S2 þ 0:035S þ 143 (14)
a suspensions on homogenisation and subsequent shearing. Food Research
At 30 °C.
complex viscosity are calculated according to the following
equations:
G00
g0 ¼
x 31–48.
G0
g00 ¼
x Biliaderis, C.G., Page, C.M., Maurice, T.J., 1986. On the multiple melting transitions of
Fig. 11 illustrates a Cole–Cole plot for PF particles in aqueous dis-
persion at 90 °C. It demonstrates a very smooth semicircular shape
of the dispersion for all particle sizes except for particles with
74 lm. The curve deviates for dispersion containing 74 lm particles
which indicates immiscibility. It is worth mentioning that the Cole–
Cole plot is not an absolute technique to determine the miscibility
of blends. Other supporting rheological data are required to
strengthen the hypothesis.
4. Conclusion
The functional properties of food powders are largely depen-
dent of the surface composition, size and surface characteristics
of the particles. Oscillatory rheology of PFD is strongly influenced
by particle size of the powders and with the sediment volume frac-
tion. The gel rigidity of the dispersion increased significantly above
the peak gelatinization temperature. The glass transition tempera-
ture and starch–lipid complex melting temperature of PF were
duly affected by particle size. The mechanical, thermal and optical
properties of PF showed reverse trends when the particle size was
reduced to 74 lm. Overall, a strong particle size dependency of PF
properties are described by a second-order polynomial equations
(Table 6). Microscopic study exhibited the disruption of cell walls
above the critical particle size limit. Since the composition of the
PF in the particles was affected by size reduction, and, therefore
further investigations are needed to establish particle size and
individual component (starch/protein/lipid) on structural property
of PF gel. These rheological and thermal properties of PF provide
important information for selecting particle size in food product
development with desired texture.
Acknowledgements
The authors express their gratitude to Kuwait University for
providing access to scanning electron microscopy equipment
(General Facility grant number GE01/07). The authors are thankful
to Dr. Vinod Kumar, Mr. Shaji Michael and Mr. Ejaj A. Bhatti, KISR
for their help in microscopy, SEM and CNS measurements.
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