Carbohydrate Polymers 65 (2006) 364–370

www.elsevier.com/locate/carbpol

Mechanism of starch gelatinization and polymer leaching

during microwave heating
T. Palav 1, K. Seetharaman *

Department of Food Science, 106 Borland Laboratory, The Pennsylvania State University, University Park, PA 16802, USA

Received 25 September 2005; received in revised form 6 January 2006; accepted 16 January 2006
Available online 12 May 2006

Abstract

The objective of this study was to investigate the process of gelatinization, granule swelling, and polymer leaching following micro-
wave heating of wheat starch suspensions. Polymer leaching was investigated as a function of heating rate, final temperature and starch
concentration. Different heating rates were achieved by changing the mass of the starch slurry heated in the microwave oven and the
temperature study was conducted on samples of same weight heated to different final temperatures. The total soluble carbohydrate
and amylose content in the supernatant was measured. Granule swelling and leaching of polymers occurred only after complete loss
of granule birefringence presenting evidence of an asynchronous process of gelatinization compared to conduction modes of heating.
The amount of soluble carbohydrate and amylose in the supernatant increased with the increase in temperature and the amylose leached
into supernatant decreased with increasing heating rates.
 2006 Elsevier Ltd. All rights reserved.

Keywords: Wheat starch; Microwave heating; Polymer leaching; Gelatinization; Granule swelling; Birefringence

1. Introduction studies that compared microwave heating to conventional

heating have been restricted to product quality attributes
Microwaves have found application in various food pro- and do not focus on the changes to starch in the system
cessing operations such as tempering, thawing, cooking, (Icoz, Sumnu, & Sahni, 2004; Martin & Tsen, 1981;
pasteurization, drying, and expansion (Decareau & Peter- Sumnu, Sahin, & Sevimli, 2005; Umbach, Davis, & Gor-
son, 1986). Microwaves are electromagnetic waves in the don, 1990). Furthermore, studies related to changes in
frequency range of 300–300,000 MHz. Polar molecules, starch granules during microwave heating in model systems
such as water or ions, absorb microwave energy and try are limited, and focus only on the comparison of granule
to orient themselves with respect to the electric field. The swelling patterns between microwave and convection heat-
rapid change in their orientation generates heat by the ed starch suspensions or starch based foods (Goebel,
molecular friction caused by disruption of weak hydrogen Grider, Davis, & Gordon, 1984; Zylema, Grider, Gordon,
bonds (Sumnu, 2001). & Davis, 1985). Studies related to starch gelatinization as
Although microwaves have many advantages, the qual- affected by microwave heating are missing in the literature
ity of products baked using microwaves are inferior com- to the best of our knowledge. This study, therefore, elabo-
pared to those baked using conventional energy sources rates on the particular differences in the mechanism of starch
(Bell & Steinke, 1991; Ovadia & Walker, 1995). Previous gelatinization by focusing on the individual events that com-
prise gelatinization when heated by using microwave energy.
*
The process of gelatinization has been extensively inves-
Corresponding author. Tel.: +1 814 865 5644; fax: +1 814 863 6132.
tigated over the past three or more decades. All of the cur-
E-mail address: Koushik@psu.edu (K. Seetharaman).
1
Current address: Rich Products Corporation, Buffalo, New York, rent understandings of gelatinization are based on heating
USA. starch granules by using conduction heating modes. Under

0144-8617/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbpol.2006.01.024
 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370 365

these conditions, gelatinization is understood as the cumu- 2.2.3. Effect of heating rate
lative irreversible changes that occur to a starch granule in The power of the microwave oven was calculated by
the presence of moisture and heat. The changes include using the following equation (Sumnu et al., 2005):
granule swelling due to absorption of moisture in the amor-
mC p DT =Dt ¼ 14:32 P ; ð1Þ
phous regions of the granule, leaching of small molecular
weight polymers including amylose, loss of the crystalline where m is the mass of sample in grams, Cp is the specific
order and the consequent loss of birefringence, leaching heat capacity of the substance in cal/g C, DT/Dt is the
of larger molecular weight polymers from the granule heating rate in C/m, and P is the power in Watts.
including fragments of amylopectin and, finally, starch sol- Based on Eq. (1), the heating rate is inversely propor-
ubilization (Atwell, Hood, Lineback, Varriano-Marston, & tional to the mass of the sample when heated in a micro-
Zobel, 1988; Leach, 1967; Olkku & Rha, 1978; Osman, wave oven. Therefore, to vary the heating rate, the
1965; Sakonidou, Karapantsios, & Raphaelides, 2003). amount of sample heated in the microwave was varied
The specific changes occur sequentially and synchronously. from 5 to 50 g. Different mass of samples of 1%, 5%, 7%
We hypothesized that the specific events of starch gelatini- or 8% starch concentration were heated in the microwave
zation during microwave heating will be different from that oven to a final temperature of 75 C. The supernatant
observed following conduction modes of heating due to was then separated and analyzed as detailed below.
the particular mechanism of heating by microwave energy.
The objective of the study therefore was to investigate the 2.2.4. Sampling and analytical techniques
mechanism of gelatinization as influenced by the starch Following different treatments, the samples were cooled
concentration, heating rate and final temperature when to 25 C and an equal amount of water at 25 C was added
heated by using microwave energy. to the sample. The samples were vortexed at low speed for
5 s and centrifuged at 2000g for 5 min. The supernatant
2. Materials and methods was then decanted and used for further analysis.

2.1. Materials 2.2.4.1. Soluble carbohydrate content. The supernatant was

analyzed for soluble carbohydrate content by using the
The wheat starch used in the study was MIDSOL-50 phenol-sulphuric acid method described by Dubois,
(Midwest Grain Products, Inc., KS, USA). Grilles, Hamilton, Rebers, and Smith (1956). All analyses
were conducted in at least duplicates and the average
2.2. Methods values are reported.

2.2.1. Heating conditions 2.2.4.2. Amylose determination. The amount of amylose

Starch samples with predetermined starch concentra- leached was determined by treating supernatant equivalent
tions were made by using wheat starch and deionized to 1 mg of soluble carbohydrates with 0.2% KI and 0.02%
water. The samples were stirred gently just before heating I2. The color developed was quantified after 20 min at
them in the microwave oven in order to ensure that the 620 nm by using a Thermo Spectronic Hekios a spectro-
starch was fully suspended in the water. A General Electric photometer. A standard curve was obtained by using the
turntable microwave (Louisville, KY, USA) oven with out- same procedure for aliquot samples of pure amylose solu-
put power 1.3 kW was used for conducting the experiments tions of known concentrations. Amylose was fractionated
in this study. In order to avoid any confounding effects due from high amylose corn starch following the procedure
to change in power absorbed due to the position of the described by Klucinec and Thompson (1998). All analyses
sample in the microwave, care was taken that the sample were conducted in at least duplicates and the average val-
was always placed at the same place within the oven. ues are reported.
Immediately following the heating treatment, sample tem-
peratures were measured by using a T-type thermocouple. 2.2.4.3. Microscopy. Treated starch samples were observed
Multiple replications were conducted in the preliminary by using light and polarized light microscope, observed
stages to determine the time required to reach specified under 40· magnification by using an Olympus BX41TF
temperatures for each treatment. The sample dimension microscope (Olympus Optical Co. Ltd., Tokyo, Japan).
and weight were chosen specifically to minimize the tem- The images were captured using SPOT Insight QE camera
perature gradient in the sample. The recorded temperatures (Diagnostic Instruments Inc., MI, USA). Samples observed
are the average sample temperatures. under light microscope were stained with vapors of Lugol’s
solution for 1–2 min based on the procedure described by
2.2.2. Effect of final temperature Hug-Iten, Escher, and Conde-Petit (2001).
A 30 g starch–water suspension at 1%, 5%, 7% or 8%
starch concentration were heated in the microwave oven to 2.2.4.4. Thermal analyses. An 8% starch sample heated to
achieve final temperatures between 60 and 95 C. The details different final temperatures was analyzed by using a Differ-
of the analysis of the supernatant are described below. ential Scanning Calorimeter (PYRIS 1 DSC, Perkin-Elmer,
366 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370

CT, USA). Approximately 20 mg of sample was weighed decrease in enthalpy between raw starch and starch heated
into a stainless steel pan and hermetically sealed. Each to 55 C and a further decrease in enthalpy at 60 C. Fur-
sample was scanned from 20 to 160 C at 10 C/min and thermore, the remnant crystals in samples heated to a final
then cooled to 20 at 10 C/min and then rescanned from temperature of 60 C melted at a higher temperature sug-
20 to 160 C at 10 C/min. An empty stainless steel pan gesting the melting of B-type starch granules.
was used as a reference. All analyses were conducted in
duplicate and the average values are reported. 3.2. Effect of final temperature and concentration

3. Results The amount of soluble carbohydrate in the supernatant

and the proportion of amylose in the supernatant as a func-
3.1. Microscopy and thermal analyses tion of final temperature are shown in Figs. 3 and 4, respec-
tively. The soluble carbohydrate content in the supernatant
Fig. 1 shows the polarized light microscope images for increased with increasing temperature at all starch concen-
raw starch and microwave-treated starches heated to final trations and the soluble carbohydrate content was lower at
temperatures of 55, 60 or 65 C. At 55 C, about half of the higher starch concentrations across all temperatures.
the starch granules exhibited birefringence, although the The increase in soluble carbohydrate content in the 1%
starch granule size did not appear to have changed. At starch suspension beyond 80 C suggests complete disinte-
60 C, only the B-type, small starch granules, exhibited gration of the granules as is also evident in the microscopic
birefringence, again with little granule swelling. At 65 C, images shown in Fig. 2c.
all starch granules lost their birefringence and the granules The proportion of amylose in the soluble carbohydrates
exhibited an increase in size. Fig. 2 shows the light micro- present in the supernatant, on the other hand, was higher
scopic images of granules heated to final temperatures of at the higher starch concentrations and increased with
65, 75, 85 or 95 C. The granules are swollen and folded increasing temperature (Figs. 4a and b). The absolute
at 65 C with little or no leachate in the suspension back- amount of amylose in the supernatant was higher at the
ground. However, with increase in temperatures beyond higher starch concentration at the lower temperature
65 C, there is significant amount of leachate in the suspen- (Fig. 4a). As the temperature increased beyond 65 C, the
sion and the granules appear ruptured with granule rem- amount of amylose in the supernatant did not increase as
nants visible. At 95 C, the granules appeared completely rapidly for the 8% starch suspension. The absolute amount
ruptured with dark clumps of staining visible. of amylose leached into the supernatant was highest for the
The gradual loss of birefringence observed by using 1% starch suspension heated to 95 C. At 95 C, almost
polarized microscopy is also reflected in the data obtained 95% of the soluble carbohydrate in the supernatant was
by using the DSC (Table 1). There is an almost 10-fold amylose in the 8% starch suspension (Fig. 4b).

Fig. 1. Polarized light microscopic images of 8% starch samples heated in microwave oven to the stated temperatures (a) raw starch; (b) 55 C; (c) 60 C;
(d) 65 C. Scale bar corresponds to 50 lm.
 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370 367

Fig. 2. Microscopic images of 5% starch sample heated in microwave oven to (a) 65 C; (b) 75 C; (c) 85 C; (d) 95 C. The starch samples have been
exposed to iodine vapor and the blue color represents amylose. Scale bar corresponds to 50 lm.

Table 1
observed for the leaching of soluble carbohydrates as a
Thermal properties of 8% starch sample heated to different final
temperatures as measured by using a differential scanning calorimeter function of heating rate with increasing starch concentra-
tion. At the 1% and 5% starch concentrations, the amount
Temperature (C) T0 (C)a Te (C)b DH (J/g)c
d
of soluble carbohydrate leached increased with increasing
Raw starch 63.5 (±0.12) 72.1 (±0.08) 12 (±0.14)
heating rate and the magnitude of increase was greater for
55 62.0 (±0.2) 76.3 (±0.1) 1.44 (±0.05)
60 66.3 (±0.09) 69.0 (±0.06) 0.43 (±0.02) the 1% starch suspension compared to 5% starch suspen-
65 –e – – sion. At 7% starch concentration, soluble carbohydrate
a
Onset temperature of gelatinization. concentration in the supernatant increased up to about
b
End temperature of gelatinization. 125 C/m heating rate after which the level of soluble car-
c
Enthalpy of gelatinization. bohydrate leached remained fairly constant. In contrast,
d
Standard deviations are indicated in parenthesis. the amount of soluble carbohydrate leached from 8%
e
No endotherm observed.
starch suspension decreased with increasing heating rates.
The proportion of amylose in the supernatant decreased
with increasing heating rate at all starch concentrations.
1% 5% 7% 8%
Furthermore, the proportion of amylose in the superna-
350
Soluble carbohydrate (mg/g of

tant was higher at the higher starch concentration

300
(Fig. 6).
250
starch)

200
4. Discussions
150

100 In a previous study in our laboratory, we observed

50 that the mechanism of heating by using microwave ener-
0
55 60 65 70 75 80 85 90 95 100
gy resulted in different gel properties when compared to
Temperature ( C)
o a conduction heated suspension (Palav & Seetharaman,
2006; manuscript in review). We proposed that the mech-
Fig. 3. Amount of soluble carbohydrates leached as a function of
temperature. The error bars show the standard deviation across measure-
anism of gelatinization due to microwave heating was
ments, but are too small be to seen. different compared to conduction heating due to both
the higher heating rates achieved and the vibrational
motion of the polar molecules due to microwave energy.
3.3. Effect of heating rate This work further investigates the leaching of polymers
and gelatinization during microwave heating as a
The heating rates achieved in the experiment ranged function of starch concentration, final temperature, and
from 90 to 350 C/m (Fig. 5). A crossover trend was heating rate.
368 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370

1% 5% 7% 8%

a b
120 100
1. 2.
90

100
Amylose in supernatant (mg/g of starch)

80

Amylose (% of soluble carbohydrates)

70
80

60

60 50

40

40
30

20
20

10

0 0
60 65 70 75 80 85 90 60 65 70 75 80 85 90
o
Temperature ( C)

Fig. 4. Amylose in supernatant represented as mg/g of starch (a) as % of soluble carbohydrate (b) as a function of temperature. Error bars denote
standard deviation of measurement but are too small.

1% 5% 7% 8% 1% 5% 7% 8%
Soluble carbohydrate (mg/g of starch)

Amylose leached (% of soluble

160 100
140 90
80
120 70
carbohydrate)

100 60
50
80 40
60 30
20
40 10
20 0
0 50 100 150 200 250 300 350 400 450
0 Heating rate ( o C/m)
0 50 100 150 200 250 300 350 400 450
Heating rate (oC/m) Fig. 6. Amount of amylose leached (% of soluble carbohydrate) as a
function of heating rate. Error bars denote the standard deviation among
Fig. 5. Amount of soluble carbohydrates in the supernatant as a function
the measurements.
of heating rate on the leaching of polymers during microwave heating.
Standard deviations among measurements are denoted by error bars.

Morrison, 1990). During conduction heating, the destruc-

4.1. Microscopy and thermal properties tion of the radial arrangement of amylopectin chains is
assisted by the swelling in the amorphous region of the
Data from the microscopic observations suggest that granule (Donald, 2004; Donovan, 1979; Jenkins & Donald,
granule swelling following microwave heating does not 1998; Tester & Morrison, 1990; Waigh, Gidley, Koman-
occur prior to the loss of birefringence (Fig. 1). This is shek, & Donald, 2000). Furthermore, the thermal analyses
the first evidence of loss of birefringence in the granules data (Table 1) obtained by using a DSC suggest that the
preceding granule swelling when heated by using micro- loss of crystalline arrangement in a microwave-heated sam-
wave energy. This behavior is different in starch suspen- ple occurs at a lower temperature compared to that
sions heated by using conduction heating wherein granule observed for conduction-heated sample. It is likely that
swelling and loss of birefringence occur almost simulta- the vibrational motion of the polar molecules during
neously (Cameron & Donald, 1993; Donald, 2004; Dono- microwave heating directly impact the crystalline lamella
van, 1979; French, 1984; Leszczynski, 1987; Tester & of the amylopectin thus disrupting the radial arrangement
 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370 369

of the amylopectin lamellae. Therefore, the crystalline 2003); i.e., the amount of microwave energy dissipated into
arrangement is destroyed prior to the glass transition of heat increases with increasing starch concentration (Buffler,
the amorphous region of the granule, thus resulting in no 1993). It is therefore likely that there is local increase in
swelling. temperature around each granule at the higher starch con-
The loss of birefringence of B-type granules occurred at centrations that potentially results in the rupture of gran-
a higher temperature compared to A-type granules. The ules; thereby increasing the local viscosity and preventing
differences in the gelatinization temperature of A- and B- leaching at higher concentrations. It is also likely that as
type wheat starch granules have been reported earlier (Kar- the initial starch concentration increases, the potential for
lsson & Eliasson, 1983) and it has also been reported that the sample to form a paste or a weak gel increases (Orford,
the crystalline region of the B-type wheat starch granules Ring, Carroll, Miles, & Morris, 1987) thereby trapping the
have greater stability compared to A-type wheat starch polymers and preventing leaching into the supernatant.
granules (Chiotelli & Le Meste, 2002; Wong & Lelievre, Starch concentrations above 6% form a gel upon cooling
1982). (Miles, Morris, Orford, & Ring, 1985). However, the 8%
At temperatures higher than 65 C, granule swelling was starch suspension in this study only formed a paste and
observed in the microwave-heated samples (Fig. 2). Gran- not a gel. Therefore, amylose does not appear to be
ule swelling was rapid following the loss of birefringence. contributing to the continuous network needed for gel
In contrast during conduction heating, swelling of granules formation following microwave heating.
and the melting of crystallites are semi-cooperative process-
es (French, 1984). At higher temperatures following micro- 4.3. Effect of heating rate solids concentration
wave heating, granular remnants, and leachate were
observed in the background suggesting rupture of granules The heating rates achieved in this study range from 90 to
due to microwave heating. This observation is also different 350 C/min and the time interval ranged from 9 to 37 s to
from that observed for starch samples heated by using con- reach a final temperature of 75 C. These heating rates are
duction heating wherein granule maintains its integrity significantly higher than what can be achieved by using
even at 90 C (Bowler, Williams, & Angold, 1982; Doubli- conduction heating. The strong interaction between initial
er, 1987; Ghiasi, Hoseney, & Varriano-Marston, 1982). starch concentration and amount of soluble carbohydrate
The rupture of the granules is also likely a function of in the supernatant is a novel observation. A starch concen-
the vibrational motion of the polar molecules during tration of 7% appears to be a critical point. It is known that
microwave heating. These observations partially explain the dielectric loss factor increases with increasing starch
the differences in the granule and gel properties of micro- concentration. It is likely that at 8% starch concentration,
wave-heated starch suspensions compared to conduction- the amount of microwave energy converted to heat (dielec-
heated samples that we reported in an earlier research tric loss factor) is significantly higher than that at lower
(Palav & Seetharaman, 2006; manuscript in review). concentrations. This would result in a very rapid increase
in the local temperature in the suspension resulting in a
4.2. Effect of final temperature and concentration rapid increase in local viscosity thus decreasing the amount
of soluble carbohydrates leached into the supernatant. The
The soluble carbohydrate content in the supernatant with proportion of amylose in the supernatant decreased with
increasing starch concentration is between 3.2 and 5.4% up increasing heating rates probably due to kinetic limitations
to about 65 C on the basis of the initial starch content at all starch concentrations. However, at higher starch con-
(Fig. 3). However, the absolute amount of amylose in the centrations, the proportion of amylose in the supernatant
supernatant at this temperature ranged from 0.4% to 2.5% was greater than that observed at the lower starch concen-
(Fig. 4a) and the relative proportion of amylose as a function trations. This is likely because the suspension following the
of the total carbohydrates in the supernatant ranged from heat treatment has a higher viscosity in the 8% suspension
8% to 78% (Fig. 4b). This corresponds to the temperature compared to the 1% suspension and the granular remnants
at which the granule birefringence was lost completely settle to the bottom leaving the amylose in the supernatant.
(65 C) and swelling was initiated (Figs. 1 and 2). Therefore,
the leaching of carbohydrates occurs only following the ini- 5. Conclusions
tiation of swelling and a higher proportion of amylose leach-
es out at the higher starch concentrations. The primary observation in this study suggests that the
At higher temperatures, the increase in the amount of gelatinization process during microwave heating is asyn-
soluble carbohydrates is dependent on the initial starch chronous compared to samples heated by using conduction
concentration in the suspension, with more carbohydrates heating. More specifically, loss of birefringence and granule
leaching into the supernatant at lower starch concentra- swelling do not occur semi-cooperatively during microwave
tions compared that observed at higher starch concentra- heating as is typical during conduction heating. The leach-
tions. It has been reported that the dielectric loss factor ing of polymers occurred only following the initiation of
of a starch suspension increases with increasing starch con- swelling as has also been shown in samples heated by con-
centration (Piyasena, Ramaswamy, Awuah, & Defelice, duction. The particular kinetics of polymer leaching was
370 T. Palav, K. Seetharaman / Carbohydrate Polymers 65 (2006) 364–370

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