Journal of Cereal Science 95 (2020) 103072

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Journal of Cereal Science

journal homepage: http://www.elsevier.com/locate/jcs

Microwave irradiation differentially affect the physicochemical properties

of waxy and non-waxy hull-less barley starch
Mengting Ma a, 1, Yu Zhang a, 1, Xiaojing Chen a, Haitao Li b, **, Zhongquan Sui a, *,
Harold Corke c, d
a
Department of Food Science & Technology, School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai, 200240, China
b
School of Food Science and Technology, Jiangnan University, Wuxi, 214122, China
c
Biotechnology and Food Engineering Program, Guangdong Technion – Israel Institute of Technology, Shantou, Guangdong, 515063, China
d
Faculty of Biotechnology and Food Engineering, Technion – Israel Institute of Technology, Haifa, Israel

A R T I C L E I N F O A B S T R A C T

Keywords: Waxy and non-waxy hull-less barley kernels and their isolated starches were irradiated under different micro­
Hull-less barley starch wave conditions (power 640, 720, and 800 W, time 60, 120 and 180 s). Changes in physicochemical properties
Microwave were studied to investigate the effects of microwave irradiation (MWI) on in-kernel starches and isolated
Gelatinization
starches. For in-kernel starch, microwave reduced the ratio of 1047/1022 cm− 1 wavelengths, gelatinization
Viscosity
enthalpy (ΔHg) and relative crystallinity (RC), indicating that microwave of starch within the cells disrupted the
crystalline regions. For isolated starch, microwave decreased the ratio of 1047/1022 cm− 1 wavelengths but
increased ΔHg of isolated starch, indicating that microwaving resulted in disruption of amorphous structure and
an increase in the amount of remaining double helix structure. Moreover, viscosities of in-kernel starches
decreased as microwave power and time increased, but this was not observed in isolated starches. Microwave
treatment induced an enhancement of gelatinization temperature for non-waxy starches (NWS) but decreased in
waxy starches (WS). Microwave had a greater effect for swelling power and solubility on in-kernel MWI-WS than
MWI-WS, whereas the reverse results were found between in-kernel MWI-NWS and MWI-NWS. The results
indicated that amylose plays a profound role in the properties of isolated and in-kernel starches during
microwaving.

1. Introduction
Hull-less barley (Hordeum vulgare L.), rich in carbohydrate, protein,
fiber, fatty acid, and β-glucan, is widely applied in the food industry,
such as for alcoholic beverages, pasta, and in baking (Abdel-Aal and
Choo, 2014). Compared with hulled barley, hull-less barley has a
recessive gene (nud), which prevents hull development (Davis et al.,
1997). The inhibition of the growth of barley husk and caryopsis is
considered an advantage in the food industry as less storage and trans­
port volume is required. In addition, vitamins and minerals are also
retained during threshing (Yangcheng et al., 2016). The content of
starch in hull-less barley kernels is 60–75% (Li et al., 2001a). Research
on hull-less barley starch is mainly promoted by scientists from China
and Canada because of its potential for production in the regions, and
have focused on comparing the properties of starches from different
cultivars. Both large lenticular granules (A-granules) of 10–25 μm in
diameter and small irregularly shaped granules (B-granules) of 2–5 μm
in diameter were observed in hull-less barley starches (Gao et al., 2009;
Kong et al., 2016). Apparent amylose content in starches extracted from
hull-less barley cultivars harvested in Canada and China varies from 0 to
39% (Abdel-Aal and Choo, 2014; Kong et al., 2016; Li et al., 2001a,
2014). Hull-less barley starch displays a typical bimodal granule-size

Abbreviations: WS, waxy hull-less barley starches; NWS, non-waxy hull-less barley starches; MWI-WS, microwave irradiated isolated waxy hull-less barley starch;
MWI-NWS, microwave irradiated isolated non-waxy hull-less barley starch; In-kernel MWI-WS, starch isolated from microwave irradiated waxy hull-less barley
kernel; In-kernel MWI-NWS, starch isolated from microwave irradiated non-waxy hull-less barley kernel.
* Corresponding author. Department of Food Science & Technology, School of Agriculture and Biology, Shanghai Jiao Tong University, Shanghai, 200240, China.
** Corresponding author. School of Food Science and Technology, Jiangnan University, Wuxi, 214122, China.
E-mail addresses: liht@jiangnan.edu.cn (H. Li), zsui@sjtu.edu.cn, springsui@gmail.com (Z. Sui).
1
Authors contributed equally to the work.

https://doi.org/10.1016/j.jcs.2020.103072
Received 15 May 2020; Received in revised form 5 August 2020; Accepted 6 August 2020
Available online 18 August 2020
0733-5210/© 2020 Elsevier Ltd. All rights reserved.
M. Ma et al.
distribution, has larger molecules of amylose and amylopectin, more­
over, the amylopectin contained a larger proportion of long chains
(Kong et al., 2016; Li et al., 2004). The physicochemical properties of
starch are controlled by its amylose content, the amylose/amylopectin
ratio and the branching structure.
In order to achieve desired physicochemical properties, native starch
can be modified in various ways. Compared with chemical and enzy­
matic techniques, physical modification is generally safer and easier to
perform. Moreover, it has sustainable and environmentally-friendly
benefits. Unlike traditional heating techniques, microwave irradiation
is based on the principle of dielectric loss. Heated materials are affected
by the electromagnetic energy from the microwave. The microwave
energy is absorbed by the polar molecules in the food material and
converted into heat energy, resulting in a rise in the temperature of the
material. Heat is generated by friction because the molecules are unable
to react instantaneously to changes in the direction of the magnetic field
(Fan et al., 2013). Microwave irradiation is gradually supplanting some
conventional processing methods due to its shorter process time, higher
yield and potentially better quality of products, and can be applied in
modified starch processing (Colman et al., 2014). Many studies have
investigated the direct effect of microwave treatment on starch prop­
erties. Shah et al. (2016) reported that microwave radiation resulted in
the development of surface cracks on Indian Horse Chestnut starch, and
viscosities and gelatinization temperatures were significantly reduced.
But Lewandowicz et al. (2000) observed that microwave radiation could
increase the gelatinization temperatures in cereal starches. The extent
and type of changes in physicochemical properties depended on the
variety of starch. However, there is limited information on microwave
irradiated hull-less barley starch. Therefore, more information needed to
explore it potential.
Some researchers concluded that the modifications of cereal starch
by microwave irradiation were analogous to those caused by heat-
moisture treatment (HMT) (Lewandowicz et al., 2000). In our previ­
ous study, the reduction in amylose leaching of in-kernel HMT rice
starch was greater than that of HMT isolated rice starch. It was postu­
lated that HMT on in-kernel starches restricted the movement of
amylose chains, leading to a more stable rearrangement within amor­
phous and crystalline domains of starch granules. Microwave irradiation
can also cause rupture and rearrangement of crystalline domains within
granules and induce breakage of glycosidic bonds, further leading to
fragmentation of starch granules (Shah et al., 2016). Up to now, there is
no specific report on direct application of microwave irradiation on
hull-less barley kernels as a function of amylose content. It was hy­
pothesized that microwave irradiation of hull-less barley starch in cells
might allow the starch chains to rupture and rearrange within crystalline
regions to a greater extent. Therefore, waxy and non-waxy hull-less
barley kernels were chosen, and the properties of in-kernel microwave
irradiated starches and microwave irradiated isolated starches were
measured. The purposes of this study were to investigate 1) the effects of
microwave (power × time) on physicochemical properties, comparing
waxy and non-waxy hull-less barley starches; 2) the difference of
properties between in-kernel starches and isolated starches during mi­
crowave process. This work will fill a gap in knowledge on microwaved
hull-less barley starches, and add to the body of knowledge on in-kernel
microwaved starches, which giving some guidance to the starch modi­
fication industry.
2. Material and methods
2.1. Materials
Waxy hull-less barley (08–1127) was provided by Tibet Academy of
Agriculture and Animal Husbandry Sciences (Tibet, China), non-waxy
hull-less barley (Tibetan short-awn white hull-less barley) was sup­
plied by Leshimai Industrial Development Co., Ltd. (Shanghai, China).
The amylose and protein contents (AACC, 2002; Method 61-03 and 46-
2
Journal of Cereal Science 95 (2020) 103072
14) of waxy and non-waxy hull-less barley kernels were 0.1%, 14%, and
11.2%, 9.9%, respectively.
2.2. Microwave irradiations on hull-less barley kernels
A microwave oven (Galanz G80F20CN2L-B8(R0), Galanz Ltd.,
China) was employed (external dimensions 0.271 × 0.45 × 0.395 m,
operating frequency of 2450 MHz). Microwave irradiation was per­
formed on hull-less barley kernels at 640 W, 720 W, or 800 W for 60 s,
120 s, or 180 s. Microwave irradiated hull-less barley kernels were
soaked in distilled water at room temperature for 10 h. Then the extra
water was discarded, the kernels were ground with NaOH solution
(0.25%, w/v) by a blender, the resulting slurry was filtrated through a
200 mesh (0.075 mm in diameter) sieve, the slurry was washed by NaOH
solution (0.25%, w/v) until no white starch washed out. The filtrate was
stored in a refrigerator at 4 ◦ C for 10 h. The filtrate was then centrifuged
at 3000×g for 15 min, the supernatant was poured out, and the top
yellow protein layer was removed using a spoon. Distilled water was
used to resuspend the lower white starch layer, the suspension was
neutralised by 0.1M HCl solution and centrifuged as above. This pro­
cedure was repeated at least three times more. The purified starch was
dried in an oven at 40 ◦ C until the moisture content of starch was
approximately 10%, and ground to pass through a 70 mesh (0.21 mm in
diameter) sieve. Starches from microwave irradiated waxy hull-less
barley kernels (in-kernel MWI-WS) and starches from microwave irra­
diated non-waxy hull-less barley kernels (in-kernel MWI-NWS) were
obtained following the above method. The purity of the isolated starches
determined by the total starch assay kit (Megazyme, Bray, Ireland) was
more than 95%.
2.3. Microwave irradiation of hull-less barley starches
Starches were extracted from untreated hull-less barley kernels ac­
cording to the above method to obtain isolated waxy hull-less barley
starch (WS) and isolated non-waxy hull-less barley starch (NWS), then
the starches were directly microwaved by a microwave oven to obtain
microwave irradiated isolated waxy hull-less barley starch (MWI-WS)
and microwave irradiated isolated non-waxy hull-less barley starch
(MWI-NWS). The conditions of microwave irradiation were three levels
of power (640 W, 720 W, and 800 W) and three levels of time (60 s, 120
s, and 180 s).
2.4. Determination of swelling power and solubility index
Starch (1 g, db) and distilled water (40 mL) were mixed in 50 mL
centrifuge tube. Then the mixture was heated for 30 min at 85 ◦ C. With a
subsequent cooling treatment, tube at room temperature was centri­
fuged for 20 min at 1000×g. The swelling power and solubility index of
starches were determined using a previously described procedure (He
et al., 2018).
2.5. Fourier transform infrared spectroscopy
The Fourier transform infrared (FT-IR) spectra of the hull-less barley
starches were recorded by a Nicolet 6700 FT-IR spectrometer equipped
with Smart iTR diamond ATR accessory (Thermo Scientific, Pittsburgh,
PA). The spectra were recorded at a resolution of 4 cm− 1 in the ranging
from 800 to 1200 cm− 1 with 128 scans. Baseline correction and
smoothing processing were applied to raw spectra by using Omnic 8.0
(Thermo Fisher Scientific., Pittsburgh, PA)
2.6. X-ray diffraction
X-ray diffraction (XRD) analyses of hull-less barley starches were
performed using the X-ray diffractometer (D/MAX-2200/PC, Rigaku
Corporation, Tokyo, Japan) equipped with a goniometer at 100 mA
M. Ma et al. Journal of Cereal Science 95 (2020) 103072

(tube current) and 40 kV (target voltage). The scanning range of the
diffraction angle (2θ) was from 5◦ to 40◦ at scanning speed of 2◦ /min
with an increment of 0.02◦ . The relative crystallinity (RC) was calcu­
lated by MDI Jade 6.5 (Materials Data., Livermore, CA) according to a
previous method (Komiya and Nara, 1986).
2.7. Determination of thermal and retrogradation properties
Sample (2 mg, db) was mixed with distilled water (6 μL) in an
aluminum pan, and equilibrated at 25 ◦ C for at least 2 h. A differential
scanning calorimeter (DSC) (TA 2910, TA Instruments, Wilmington, DE)

Fig. 1. The swelling power (g/g) and the solubility (%) of native and microwave irradiated hull-less barley starches. The error bars are based on three tech­
nical repeats.

3
M. Ma et al.
was used to measure the thermal properties of the samples using a
previously described procedure (Sui et al., 2017).
2.8. Determination of pasting properties
The pasting properties of hull-less barley starches were measured by
a Rapid Visco Analyser (RVA) (Newport Scientific, Warriewood,
Australia) following the method described by Zhan et al. (2020). Starch
(3 g, db) was weighed in an aluminum container, then distilled water
was added to reach a total weight of 28 g. The heating and cooling
program were set as follows: the temperature of samples was equili­
brated at 50 ◦ C for at least 1 min, the plastic paddle was stirred at the
rate of 960 r/min for 10 s to evenly blend the starch-water mixture. Then
the stirring rate was reduced to 160 r/min and kept until the end of the
program. The mixture was heated from 50 ◦ C to 95 ◦ C at the rate of 6
◦
C/min and held at 95 ◦ C for 5 min. After that, the temperature
decreased from 95 ◦ C to 50 ◦ C in 7.5 min and was then held at 50 ◦ C for
2 min.
2.9. Statistical analysis
Data from three technical replications were presented as mean ±
standard deviation. A one-way Analysis of Variance (ANOVA) with
Duncan’s multiple comparison test was used to determine the statisti­
cally significant differences in the means. These analyses were computed
with SPSS 17.0 (SPSS., Chicago, IL).
3. Results and discussion
3.1. Swelling power and the solubility index
The swelling power (SP) and solubility index (SOL) of native and
microwave irradiated hull-less barley starches (Fig. 1) show that the
amylose content of starch restricts granular swelling behavior. WS
exhibited higher SP but lower SOL than NWS, which was in line with
previous reports (Li et al., 2001b). Swelling power is primarily influ­
enced by amylopectin while the amylose content influences solubility
(Li et al., 2014). WS granules with a less rigid structure were more easily
swollen and ruptured. In contrast, NWS granules were less swollen and
tended to retrograde easily.
The SP values of in-kernel MWI-WS and MWI-WS decreased with
increasing microwave conditions (power × time) to a different extent.
During the microwave process, the partially degraded amylose and
amylopectin chains in starch molecules increased the proportions of
short chains. This phenomenon is negative for granule swelling (Zeng
et al., 2016). Li et al. (2019) also observed that SP of millet starch
generally decreased with the increase of microwave time. The reduction
in SP values of in-kernel MWI-WS was more intense possibly resulting
from the degradation of starch molecules to a greater extent. However,
the SP values of in-kernel MWI-NWS were slightly higher than those of
native NWS. A similar trend in MWI-NWS was observed for SP values,
whereas the extent of change in MWI-NWS was greater than in-kernel
MWI-NWS following microwaving to 60 s, 120 s, and 180 s. The oppo­
site effect of microwave irradiation on SP values of WS and NWS may be
due to many factors (e.g., amylose content, amylopectin structure,
crystalline regions). The changes in starch swelling after microwave
irradiation may due to the rearrangement of crystalline regions within
the granules, then the internal distribution within starch granules be­
comes more random (Luo et al., 2006).
With increasing microwave power and time, the SOL values of in-
kernel MWI-NWS and in-kernel MWI-WS were appreciably enhanced,
and microwave time had a more pronounced effect on the SOL values
than did power. Upon microwave irradiation, the SOL values of starch
increased due to the decrease of inter chain hydrogen bonds and an
increase of hydrogen bonds with water (Shah et al., 2016). As micro­
wave time increased, the SOL values of MWI-NWS increased at lower
4
Journal of Cereal Science 95 (2020) 103072
power, but decreased at higher power. The SOL values of MWI-WS were
lower than that of native WS, with the exception of the SOL of MWI-WS
microwave irradiated at 800 W and 180 s. The characteristics of amylose
and amylopectin influence starch solubility, including the ratio of
amylose to amylopectin, the molecular weight distribution, degree/­
length of branching, and conformations of molecules, etc. (Gani et al.,
2014).
Changes in SP and SOL values between in-kernel microwave irradi­
ated starches and microwave irradiated isolated starches were related to
the presence of amylose. The changes in SP and SOL of in-kernel MWI-
NWS were less intense than MWI-NWS, which suggested that microwave
irradiation had less impact on in-kernel NWS than isolated NWS. This
phenomenon indicated that microwave irradiation within non-waxy
hull-less barley kernels restricted amylose chains movement, resulting
in a more effective rearrangement within amorphous and crystalline
domains of starch granules confined within the cells so that swelling and
any displacement of molecules within the granules would be limited. Sui
et al. (2017) also found that HMT of in-kernel rice starches had a less
effect on SP and SOL than that of isolated starches.
The impact of microwave on in-kernel NWS was less than in-kernel
WS, which may be explained by amylose acting as a diluent or an in­
hibitor (He et al., 2018). Interestingly, microwave had a pronounced
effect of SP and SOL on in-kernel MWI-WS than MWI-WS. It was pre­
sumed that high-energy microwaves could cause intense movement and
disruption of the starch molecular chain, so isolated WS without
amylose had relative freedom; it could flexibly absorb the energy of
microwave while avoiding destruction of the starch molecule. In-kernel
WS limited by other component molecules (e.g., protein) which could be
damaged by receiving the high energy. Thus, the effect of microwave
irradiation on in-kernel WS was larger than on isolated WS. However,
when amylose chains were present in starch, the amylose molecules may
provide the linkages between broken amylopectin clusters. Fixed starch
molecules directly irradiated by microwave, will receive all the energy,
thus, molecules will break. So, the impact of microwave irradiation on
isolated NWS was greater than in-kernel NWS.
3.2. Fourier transform infrared spectroscopy (FT-IR)
In Fourier infrared spectra, the peak absorption value at 1047 cm− 1
wavelength is related to the crystalline order, while the peak value at
1022 cm− 1 reflects the amorphous regions of starch (Wang et al., 2017).
Therefore, the ratio of amplitudes of absorbance at 1047 and 1022 cm− 1
can be used as an indicator of the ratio of ordered crystalline regions to
amorphous regions within the starch granule or the short-range mo­
lecular order for starches (van Soest et al., 1995). A higher ratio in­
dicates higher short-range order and larger crystalline region of starch.
The ratios of 1047/1022 cm− 1 intensity for native and microwave
irradiated hull-less barley starches are depicted in Fig. 2. The ratios in
native NWS and WS were 0.49 and 0.50. The short-range order is related
to amylopectin content. With higher content of amylopectin, more
crystalline structure and higher short-range molecular order occurs in
starch granules. The ratios of 1047/1022 cm− 1 of all microwave irra­
diated samples (in-kernel MWI-NWS, MWI-NWS, in-kernel MWI-WS and
MWI-WS) decreased to different extents. It indicated that microwave
irradiation might damage to the conformation of hull-less barley starch,
including the structure of the double helices and crystalline domains,
which are reflected in the decrease of the short-range order and relative
crystallinity (long-range molecular order). (Li et al., 2019).
3.3. X-ray diffraction
All hull-less barley starches displayed typical A-type polymorphs
(Fig. 3), which showed two single broad peaks at 15◦ , 23◦ (2θ), and dual-
peaks at 17◦ and 18◦ (2θ), indicating that microwave irradiation did not
alter the crystalline pattern of hull-less barley starch. There was an
additional diffraction peak at 20◦ (Fig. 3) due to the amylose-lipid
M. Ma et al.
Fig. 2. Short range molecular orders (Ratios of 1047/1022 cm− 1) of native and microwave irradiated hull-less barley starches by FT-IR. The error bars are based on
three technical repeats.
complex (Yangcheng et al., 2016), but hardly observed in WS due to the
absence of amylose. The stronger microwave treatment on NWS did
decrease the intensity of the diffraction peak at 20◦ , suggesting that the
amylose-lipid complex was hard to form when NWS was irradiated
under strong microwave conditions. Relative crystallinity (RC) values of
WS and NWS were 26.97% and 20.63%, similar to the results of Yang­
cheng et al. (2016) and within the range of RC reported for hull-less
barley starch (Li et al., 2014). These results were consistent with
amylose contents were being negatively correlated with RC (Cai et al.,
2015). The differences in RC of hull-less barley starches may be due to a
variety of factors. According to Wongsagonsup et al. (2008), the crys­
talline structure of starch is related to many factors, including amylo­
pectin content, amylopectin chain-length distribution, the orientation of
the double helices within the crystalline area and weight ratio of
amylopectin short chains.
Notably, microwave irradiation induced the reduction of RC values
for all starches. This phenomenon might be attributed to the movement
of double helices, which could disrupt starch crystallites and change
crystalline orientation, owing to the microwave treatment (Wang et al.,
2019). As the microwave condition (power × time) increased, the RC
values of in-kernel MWI-NWS and in-kernel MWI-WS decreased,
whereas the values of MWI-NWS and MWI-WS increased. The more
damaged internal crystalline structure occurred in in-kernel starches
with the stronger microwave conditions. Absorbed microwave energy in
hull-less barley kernel is converted into kinetic energy, which causes the
starch molecules to vibrate rapidly and generate heat by friction. The
generated heat increases the system temperature, and when it reaches
the gelatinization temperature, the starch begins to gelatinize, resulting
in the decrease in crystallinity (Tao et al., 2020). In contrast, double
helices with the relative freedom of isolated starches can be flexible to
5
Journal of Cereal Science 95 (2020) 103072
avoid the damage, so that microwave irradiation destroyed the amor­
phous region more than the crystalline region. On microwave irradia­
tion, recrystallization occurred in the loose structure of starch segment
within the crystalline domain, which resulted in an increase of relative
crystallinity (Fan et al., 2013).
3.4. Thermal and retrogradation properties
WS showed higher gelatinization temperatures (To, Tp and Tc) than
NWS (Table 1), which was in agreement with the previous report about
waxy and normal hull-less barley starch (Li et al., 2001b). It indicated
that a considerable amount of energy is required for WS gelatinization.
This results from the fact that WS had a higher proportion of long-chain
branches, leading to producing stronger crystallization in the starch
chain, requiring more energy to unravel and melt its double helices (Zhu
et al., 2011). By comparison, NWS had higher proportions of short-chain
branches that were too short to form stable double helices and required
less energy for gelatinization (Bao et al., 2006). Except in amylopectin
branch chains, amylose content, amylose-lipid complexed chains and
the molecular architecture of the crystalline region can influence the
gelatinization temperatures (Ma et al., 2017).
Microwave irradiation increased gelatinization temperatures (Tp, Tc
and Tc–To) of NWS to a different extent (Table 1), except for microwave
irradiated isolated NWS at 800 W and 180 s respectively. This increase
could be explained by enhanced interactions among the starch chains in
amorphous regions. The results were consistent with previous reports
that the gelatinization temperatures of maize starches are increased by
microwave treatment (Luo et al., 2006). Li et al. (2019) believed that in
the microwave processing, hydration breaks down the inter- and
intra-molecule hydrogen bonding and the hydrogen bonds between
M. Ma et al.
Fig. 3. XRD patterns of native and microwave irradiated hull-less barley starches. XRD calculations are within standard deviations of 2%.
water and starch molecules are regenerated. These changes enhance the
hydrogen bonding in the molecules, which are also reflected by
increased gelatinization temperature. An interesting phenomenon was
that microwave irradiation induced a significant reduction of isolated
and in-kernel WS for To and Tp, which might be explained gelatinization
causing a partial loss in molecular order and crystalline structure
resulting from microwave treatments (Shah et al., 2016). Gelatinization
temperature is negatively correlated with the proportion of short branch
chains (DP 6–12) of amylopectin and positively correlated with the
proportion of long branch chains (DP > 36). Therefore, the decrease of
gelatinization temperature in MWI-WS and in-kernel MWI-WS may be
attributed to the rupture of chains, an increase of short branch chains of
amylopectin, and a decrease of long branch chains of amylopectin
during microwave process. The short-chain branch of amylopectin de­
stroys the stability of the crystal layer structure, while the long-chain
branch of amylopectin can form a long double helix, requiring a
higher temperature to completely dissociate (Park et al., 2007).
The gelatinization enthalpy (ΔHg) reflects the melting of double
helices and the energy requirement of starch for gelatinization. The ΔHg
of a transition corresponds to the degree of crystal order (or double-
helical structure) in the starch suspensions (Cooke and Gidley, 1992).
With increasing microwave power and time, the ΔHg values in MWI-WS
and MWI-NWS increased, indicating disruption of amorphous structure
and increase in the level of remaining double helix structure (Li et al.,
2019). The decrease in ΔHg values for in-kernel MWI-WS and in-kernel
MWI-NWS suggested that some of the double-helical structure present in
crystalline regions of the granule may have been destroyed under the
prevailing conditions during microwave irradiation. The crystalline
domain is more resistant to modification than the amorphous domain
because of the ordered structure. The change in ΔHg reflected that mi­
crowave irradiation had more effect on the starch structure of in-kernel
starch than isolated starch. Microwave treatment of hull-less barley
6
Journal of Cereal Science 95 (2020) 103072
starch within the cells had the greater effect on the degree of disruption
of amylopectin clusters in the crystalline regions, which was in line with
previously reports that HMT exhibited a more pronounced impact on
in-kernel rice starches than rice starches (Sui et al., 2017). The retro­
gradation enthalpy (ΔHr) of all starches after storage in 4 ◦ C for 7 days
were analyzed by rescanning the samples with DSC. ΔHr of MWI-WS and
MWI-NWS increased during microwaving, which resulted from
increased crystallinity, and decreased the degree of separation between
the outer branches of adjacent amylopectin chain clusters (Kong et al.,
2015). It also suggested that hull-less barley starch retrograded to a
greater extent after microwave irradiation.
3.5. Pasting properties
The pasting curve is one of the most important indicators of struc­
tural and functional properties of starch, and subtle changes in inter­
molecular conformation can lead to significant changes in pasting
behaviour (Li et al., 2019). Pasting curves of starches before and after
microwave irradiation are presented in Fig. 4. The viscosities increased
for NWS curves and decreased for WS curves during the cooling process.
During microwave treatment, the change in viscosities of in-kernel
starches were greater than those of isolated starches, and greater
changes of viscosities occurred in NWS compared with WS. This result is
in good agreement with a previous study that the extent of change in the
pasting properties of in-kernel HMT starches was greater than those of
HMT isolated starches (Sui et al., 2017).
Pasting curves of all starches had a clear peak viscosity (PV). PV
reflects the ability of starch to bind water and the maximum swelling of
the starch granule before its disintegration (Ma et al., 2017). Under
microwave irradiation, the reduction in PV of in-kernel MWI-WS
exhibited a similar trend to in-kernel MWI-NWS (Table 2). PV of
in-kernel starches significantly decreased with the increase of
M. Ma et al. Journal of Cereal Science 95 (2020) 103072

Table 1
Thermal and retrogradation properties of native and microwaved hull-less barley starches.
Samples Treatment To (◦ C) Tp (◦ C) Tc (◦ C) Tc–To (◦ C) ΔHg (J g− 1) △Hr (J g− 1)

Microwave time Microwave power

(s) (W)

In-kernel MWI- 0 0 54.58 ± 58.46 ± 0.11jk 62.68 ± 0.02f 8.10 ± 0.00j 10.65 ± 0.47d 3.24 ± 0.01h
NWS 0.02ghij
60 640 54.80 ± 59.21 ± 63.90 ± 0.70cd 9.10 ± 0.51fgh 10.26 ± 0.91de 3.66 ± 0.08ef
0.19ghi 0.47ghi
720 54.84 ± 0.28gh 59.26 ± 0.32gh 63.49 ± 0.52de 8.66 ± 0.25hij 8.75 ± 1.78ef 3.59 ± 0.02ef
800 54.05 ± 0.20k 58.82 ± 0.23ij 63.51 ± 0.07de 9.46 ± 0.13defg 8.28 ± 0.14f 3.22 ± 0.04h
120 640 54.24 ± 0.15jk 59.18 ± 0.10hi 63.91 ± 0.08cd 9.67 ± 0.07cdef 8.61 ± 0.04ef 3.21 ± 0.02h
720 54.21 ± 0.08jk 59.40 ± 0.13gh 64.13 ± 0.77bcd 9.92 ± 0.85bcd 9.61 ± 0.61def 3.42 ± 0.01g
800 54.52 ± 0.08hij 59.64 ± 0.06fg 64.31 ± 0.09abc 9.79 ± 0.01bcde 8.62 ± 0.01ef 3.70 ± 0.06e
180 640 54.45 ± 0.06ij 59.97 ± 0.04ef 64.73 ± 0.12ab 10.28 ± 0.06bc 10.67 ± 0.12d 4.05 ± 0.09d
720 54.51 ± 0.08hij 59.85 ± 0.29ef 64.89 ± 0.25ab 10.28 ± 0.06b 10.70 ± 0.18d 3.51 ± 0.11fg
800 54.58 ± 60.13 ± 0.20de 65.00 ± 0.54a 10.42 ± 0.33b 10.45 ± 0.67d 2.99 ± 0.03i
0.21ghij
MWI-NWS 60 640 56.27 ± 0.00a 61.06 ± 0.07a 64.64 ± 0.18ab 8.37 ± 0.18hij 13.38 ± 0.32bc 4.02 ± 0.07d
720 56.09 ± 0.22ab 60.85 ± 0.06ab 64.84 ± 0.27ab 8.76 ± 0.49hij 13.11 ± 0.34c 4.54 ± 0.22b
800 56.12 ± 0.22ab 60.78 ± 0.29ab 65.05 ± 0.37a 8.93 ± 0.16ghi 13.40 ± 0.45bc 4.22 ± 0.02c
120 640 55.87 ± 0.09bc 60.75 ± 0.08ab 64.94 ± 0.13a 9.07 ± 0.23fgh 12.76 ± 0.16c 4.04 ± 0.00d
720 55.64 ± 0.06cd 60.56 ± 64.34 ± 0.07abc 8.71 ± 0.01hij 14.32 ± 1.72abc 4.37 ± 0.00c
0.08bcd
800 55.43 ± 0.11de 60.61 ± 0.19bc 64.46 ± 0.22abc 9.03 ± 0.11fghi 14.21 ± 0.30abc 4.31 ± 0.01c
180 640 55.19 ± 0.10ef 60.44 ± 64.48 ± 0.07abc 9.29 ± 14.94 ± 0.44ab 4.73 ± 0.04a
0.02bcd 0.03defgh
720 54.93 ± 0.21fg 60.18 ± 64.10 ± 0.11bcd 9.17 ± 0.11efgh 15.20 ± 0.89a 4.05 ± 0.01d
0.07cde
800 51.08 ± 0.27l 58.07 ± 0.01k 62.97 ± 0.09ef 11.89 ± 0.18a 13.12 ± 0.59c 3.52 ± 0.08fg
a a f efg
In-kernel MWI-WS 0 0 59.91 ± 0.12 66.47 ± 0.10 71.11 ± 11.21 ± 0.50 16.37 ± 1.21 3.40 ± 0.08e
0.62abcde
60 640 59.55 ± 0.13a 66.02 ± 0.02a 71.21 ± 0.11abcd 11.66 ± 0.02f 15.64 ± 0.96gh 3.34 ± 0.13e
720 59.50 ± 0.19a 65.49 ± 0.02cd 71.35 ± 0.28ab 11.86 ± 0.09f 15.92 ± 0.81fgh 3.45 ± 0.07e
800 59.61 ± 0.36a 65.83 ± 0.21bc 70.25 ± 10.65 ± 0.50f 17.01 ± 3.70 ± 0.38de
0.86abcde 0.23defg
120 640 56.75 ± 0.16e 64.28 ± 0.59hi 71.98 ± 0.78a 15.23 ± 0.95c 15.49 ± 1.67gh 5.01 ± 0.24a
720 55.65 ± 0.16f 64.15 ± 0.07i 70.65 ± 15.00 ± 0.78c 12.37 ± 0.54i 3.92 ±
0.93abcde 0.01cde
800 56.52 ± 0.34e 64.66 ± 0.00gh 70.95 ± 14.43 ± 0.28cd 12.89 ± 0.02i 3.91 ±
0.06abcde 0.00cde
180 640 55.13 ± 0.45f 64.00 ± 0.17i 70.86 ± 0.66bcde 15.73 ± 0.21c 13.93 ± 1.48hi 4.38 ± 0.01bc
720 53.23 ± 0.04g 63.24 ± 0.08j 71.18 ± 1.07abcd 17.95 ± 1.03b 12.79 ± 1.11i 4.05 ± 0.12cd
800 50.58 ± 0.29h 62.17 ± 0.21k 71.28 ± 1.57abc 20.71 ± 1.86a 13.74 ± 0.85hi 3.57 ± 0.06de
MWI-WS 60 640 58.94 ± 0.10b 65.28 ± 0.09de 70.06 ± 0.03bcde 11.12 ± 0.13f 18.75 ± 0.72bcd 5.01 ± 0.01a
720 58.94 ± 0.10bc 64.82 ± 0.25fg 70.63 ± 12.01 ± 0.91ef 18.18 ± 4.74 ± 0.01ab
1.00abcde 0.08cdef
800 58.66 ± 0.26bc 65.35 ± 0.13de 69.64 ± 0.47bcde 10.98 ± 0.21f 18.61 ± 4.69 ± 0.02ab
1.02bcde
120 640 58.35 ± 0.06cd 64.92 ± 69.77 ± 0.04bcde 11.42 ± 0.03f 19.01 ± 0.72bcd 5.03 ± 0.01a
0.13efg
720 58.64 ± 0.07bc 64.74 ± 0.00fg 69.78 ± 0.05bcde 11.14 ± 0.02f 19.46 ± 0.16bc 4.07 ± 0.02cd
800 58.22 ± 0.13cd 65.15 ± 69.42 ± 0.64de 11.20 ± 0.51f 19.92 ± 0.39bc 3.73 ± 0.00de
0.03def
180 640 58.20 ± 0.33cd 65.33 ± 0.23de 69.35 ± 0.32e 11.15 ± 0.64f 22.74 ± 0.78a 3.75 ± 0.02de
720 57.95 ± 0.52d 64.92 ± 69.50 ± 1.34cded 11.55 ± 0.81f 18.04 ± 4.51 ±
0.13efg 2.46cdef 0.10abc
800 56.76 ± 0.27e 64.29 ± 0.16hi 70.14 ± 0.35bcde 13.38 ± 0.08de 20.77 ± 0.69ab 4.72 ± 0.03ab

Data from three technical replications were presented as mean ± standard deviation.
Values in each column (within the same cultivar) with different superscripts are significantly different (p < 0.05).
To, onset gelatinization temperature; Tp, peak gelatinization temperature; Tc, conclusion gelatinization temperature; Tc–To, gelatinization temperature range; ΔHg,
gelatinization enthalpy; ΔHr, retrogradation enthalpy.

microwave power and time. A similar phenomenon for PV of millet
starch under microwaving has been reported (Li et al., 2019). After
microwave treatment, the breakage of the starch chains and weaker
interaction forces among the starch molecules would occur, which leads
to a reduction in viscosity (Hu et al., 2019). During the microwave
process, polar components (such as water) vibrate rapidly, the friction
and collision between water molecules and starch granules increases the
temperature in a short time, which causes physical damage to the
granules, and degrades the molecular structures of starch (Zeng et al.,
2016). The lowest values of PV occurred for in-kernel WS and NWS after
180 s microwaving at 800 W. The degree of change in the viscosity for
in-kernel MWI-NWS was greater than in-kernel MWI-WS, which indi­
cated more serious damage to granule structure of the in-kernel NWS
than in-kernel WS.
PV of MWI-NWS increased with increasing power at short times (60 s
and 120 s), yet decreased with increased power at the long time (180 s).
MWI-NWS after 180 s microwaved at 800 W showed the lowest PV
values. There was no doubt that strong microwave treatment converted
more electromagnetic energy into thermal energy, which brings more
damage to starch granule (Fan et al., 2013). As the microwave power
increased, thermal energy increased, the extent of dilatancy increased,
shortly afterward, the dilatancy disappeared, a greater extent of starch

7
M. Ma et al.
Fig. 4. RVA curves of native and microwave irradiated hull-less barley starches.
disruption occurred, and amylose chains and amylose-lipid networks
were broken (He et al., 2018). This process leads to first increasing and
then decreasing PV values. However, all MWI-WS showed higher PV
than native WS. Some researchers have revealed that microwaves can
break the linkages of starch molecules rather than merely causing them
to vibrate. Yang et al. (2017) claimed that the degree of branching of
microwaved waxy maize starch decreased with the duration of micro­
wave treatment, indicating that the amount of α-1,6-glycosidic linkages
decreased. Zhong et al. (2019) reported that short amylopectin chains
(DP 6–36) and intermediate amylose chains (DP 150–2000) of
high-amylose maize starch were partially broken under microwaving.
Shah et al. (2016) believed that a reduction in PV resulted from the
degradation of polysaccharide and a decrease in swelling power. The
degraded molecules of in-kernel starch have been attributed to micro­
wave energy, whereas molecular chains of WS were only flexed, not
disintegrated by microwave irradiation. Because of the existence of
amylose chains, fixed molecules of NWS could be degraded under
stronger microwave conditions. The differences of PV in MWI-WS and
MWI-NWS were consistent with the results for swelling power, further
supporting the above hypothesis.
Breakdown is the measure of the disintegration degree of starch
granules. During breakdown, swollen granules are disrupted and the
molecules of amylose will leach out. Setback reflects the tendency to
retrograde in the starch granules (Zaidul et al., 2007). The low viscos­
ities of starch microwaved at 800 W for 180 s among in-kernel
MWI-NWS were in accordance with high Tp and Tc and low ΔHr
values, which indicated the microwaved starch granules had thermal
stability and low tendency of retrogradation. WS, lacking amylose,
exhibited lower setback viscosities than NWS. Kong et al. (2016)
observed that the pasting properties of hull-less barley starch were
inversely correlated with amylose content, and influenced by amylo­
pectin structure among different barley varieties.
8
Journal of Cereal Science 95 (2020) 103072
4. Conclusion
Microwave irradiation altered the physicochemical properties of
isolated and in-kernel hull-less barley starches as a function of micro­
wave power and time. Changes were significantly different due to mi­
crowave irradiation on starch properties comparing isolated and in-
kernel hull-less barley starches and between non-waxy starch and
waxy starch. Microwave induced the damage to the conformation of all
starches reflected by decrease in the ratio of 1047/1022 cm− 1 wave­
lengths. Microwave increased SP and gelatinization temperature in non-
waxy starch but reduced them in waxy starch. As microwaving
increased, RC and ΔHg of in-kernel starches decreased, whereas the
values for isolated starches increased. Viscosities of in-kernel starches
decreased as microwaving increased, but this was not observed in iso­
lated starches. These results suggested that microwaving of starch
within the cells might have the greater effect on the degree of disruption
of amylopectin clusters in the crystalline regions. Future work is
necessary to characterize fine structure of isolated and in-kernel starches
during microwaving and analyze their relationship with physicochem­
ical properties.
CRediT authorship contribution statement
Mengting Ma: Data curation, Formal analysis, Writing - original
draft, Writing - review & editing. Yu Zhang: Conceptualization, Inves­
tigation, Methodology, Data curation, Formal analysis. Xiaojing Chen:
Investigation, Methodology, Data curation. Haitao Li: Conceptualiza­
tion, Investigation, Methodology, Writing - original draft, Writing - re­
view & editing. Zhongquan Sui: Conceptualization, Investigation,
Methodology, Project administration, Supervision, Writing - review &
editing. Harold Corke: Writing - review & editing.
M. Ma et al. Journal of Cereal Science 95 (2020) 103072

Table 2
Pasting properties of native and microwaved hull-less barley starches.
Samples Treatment Peak viscosity (mPa⋅s) Breakdown (mPa⋅s) Final viscosity (mPa⋅s) Setback (mPa⋅s)

Microwave time (s) Microwave power (W)

In-kernel MWI-NWS 0 0 1704±6c 365±1fjhi 3387 ± 18de 2048 ± 11ef

60 640 1651 ± 10cd 376±4efjhi 3039±6f 1764±1g
720 1540±2e 393±3defgh 3884±8b 2737±8b
800 1508±3ef 358±4ghi 3805±8bc 2655±7b
120 640 1478±6f 467±2c 3244±1ef 2233±8de
720 1333±3g 474±5c 2717 ± 18g 1857 ± 20fg
800 1252 ± 11h 487±2c 2153±1h 1388±9h
180 640 944±8j 434±1cdef 1253±8i 743 ± 16i
720 744 ± 11k 353±9hij 933±5j 542±3ij
800 550±4l 290±1j 639±2k 379±1j
MWI-NWS 60 640 1678 ± 23cd 444 ± 59cde 3574 ± 206cd 2339 ± 242cd
720 1699 ± 30c 454 ± 43cd 3791 ± 188bc 2546 ± 202bc
800 1865±6b 613 ± 28b 4385 ± 231a 3133 ± 253a
120 640 1892 ± 71ab 676 ± 72ab 4464 ± 177a 3248 ± 178a
720 1905 ± 69ab 685 ± 55a 4367 ± 67a 3147 ± 54a
800 1945 ± 18a 708±5a 4458 ± 13a 3221 ± 25a
180 640 1536±4e 366±2fghi 3422±8de 2252±3de
720 1632 ± 37d 429 ± 37cdefg 3776 ± 107bc 2573 ± 107bc
800 1025±4i 306 ± 52ij 2110 ± 285h 1391 ± 236h

In-kernel MWI-WS 0 0 2071 ± 48h 1490 ± 68e 743 ± 22abc 162 ± 12ef
60 640 2168 ± 13f 1576±6c 774±1abc 182 ± 21cde
720 2194±6ef 1553 ± 13cd 822±1a 181±8cde
800 2118±6g 1501±8de 796 ± 11ab 179 ± 13de
120 640 1800±6i 1162 ± 10f 791±1ab 153±3ef
720 1716±8j 1054±8g 823±4a 161±4ef
800 1624±6k 954±8h 823±4a 154±6ef
180 640 1560 ± 32l 873±9i 844 ± 21a 157 ± 21ef
720 1282±6m 582±5j 848±2a 147±1ef
800 891±7n 361±1k 669±4c 139±2f
MWI-WS 60 640 2205±7def 1653 ± 27ab 703 ± 152bc 228±3ab
720 2215 ± 29cdef 1636 ± 18b 804±9ab 225±1ab
800 2222 ± 37cde 1648 ± 35ab 803±1ab 229±1ab
120 640 2255 ± 12bcd 1648 ± 44ab 842 ± 10a 236 ± 22ab
720 2239 ± 40bcde 1649±8ab 818 ± 37ab 227 ± 10ab
800 2261±5abc 1658±4ab 817 ± 15ab 214±6abc
180 640 2286±9ab 1706±8a 829±1a 249±2a
720 2285±8ab 1671±6ab 816±8ab 202±7bcd
800 2307 ± 18a 1666 ± 32ab 849 ± 35a 207 ± 48bcd

Data from three technical replications were presented as mean ± standard deviation.
Values in each column (within the same cultivar) with different superscripts are significantly different (p < 0.05).

Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Acknowledgements
This research was financially supported by the National Natural
Science Foundation of China (31671893, 81402366, 81773064), the
National Key R&D Program of China (2016YFD0400206). The authors
thank Tashi Norbu of Tibet Academy of Agriculture and Animal Hus­
bandry Sciences for providing waxy hull-less barley.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.jcs.2020.103072.
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