LWT - Food Science and Technology 62 (2015) 319e324

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LWT - Food Science and Technology

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

Effect of heat-moisture treatment with maltitol on physicochemical

properties of wheat starch
Qingjie Sun*, Chong Nan, Lei Dai, Liu Xiong
College of Food Science and Engineering, Qingdao Agricultural University, Qingdao, Shandong Province, 266109, China

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 29 August 2013
Received in revised form
27 November 2014
Accepted 16 January 2015
Available online 24 January 2015

Effect of heat-moisture treatment (HMT) with maltitol on physicochemical properties of wheat starch
was investigated. Compared with the mixture of maltitol and wheat starch (MAWS), peak viscosity,
trough viscosity, nal viscosity, breakdown and setback of MAWS modied by heat-moisture treatment
(HMT-MAWS) was decreased by 119.29, 63.37, 84.50, 55.92, 21.12 RVU, respectively. The viscosities of
HMT-MAWS were affected more remarkably than that of the mixture of maltitol and heat-moisture
treatment modied wheat starch (MA-HMTWS). Gelatinization temperature (To, Tp, Tc) of HMTMAWS increased signicantly than that of MAWS. Scanning electron microscope showed that a layer
of membrane-like substance adhered to the smooth surface of HMT-MAWS, but that of MAWS became
rough with a lot of small particles. After gelatinization and freeze drying, the gel structure of HMT-MAWS
was tighter than that of MAWS. According to X-ray diffraction pattern, the area of amorphous region of
HMT-MAWS was higher than that of MAWS.
2015 Elsevier Ltd. All rights reserved.

Keywords:
Maltitol
Wheat starch
Physicochemical properties
Heat-moisture treatment

1. Introduction
Starch is the main polysaccharide in plant-origin food products.
It is commonly used as thickener, colloidal stabilizer, gelling,
bulking and water preserving agent. The granule swelling, gelatinization, pasting and the subsequent gel properties of starch play
important roles in the food manufacturing industry. With the use of
starch in food industry becoming increasingly broader and more
extensive, native starch does not always possess the physicochemical properties appropriate for certain types of processing.
Starch is often modied by physical, chemical, and enzymatic
processes to promote specic functional properties. Heat-moisture
treatment (HMT) is one of the more important physical methods by
using simple and environmentally safe processes, with low cost and
without by-products of chemical reagents (Adebowale, OluOwolabi, Olayinka, & Lawal, 2005; Sun, Wang, Xiong, & Zhao,
2013; Zavareze & Dias, 2011). HMT involves treatment of starch
granules at low moisture levels (<35 g/100 g) within a certain time
period (15 mine16 h) and at a specic range of temperature
(84e120
C) above the glass transition temperature but below the

* Corresponding author. The School of Food Science and Engineering, Qingdao

Agricultural University, 266109, 700 Changcheng Road, Chengyang District, Qingdao, China. Tel.: 86 532 88030448; fax: 86 532 88030449.
E-mail address: phdsun@163.com (Q. Sun).
http://dx.doi.org/10.1016/j.lwt.2015.01.027
0023-6438/ 2015 Elsevier Ltd. All rights reserved.

gelatinization temperature (Gunaratne & Hoover, 2002; Hoover &

Vasanthan, 1994; Takaya, Sano, & Nishinari, 2000).
Additives such as sugar are commonly used in starch-based
foods in order to optimize the processing operation and enhance
food quality by inuencing the gelatinization and retrogradation of
starch. However, food high in sugar and calories can lead to diseases
such as obesity and diabetes. In recent times, people pay more
attention to healthy eating habits and low-calorie diets. The possibility of using sugar alcohol instead of sucrose as a sweetener has
attracted more and more researchers' attention (Kommineni,
Amamcharla, & Metzger, 2012; Lin, Lee, Mau, Lin, & Chiou, 2010).
Maltitol, a sugar alcohol used to replace table sugar as a sugar
substitute, has fewer calories, does not promote tooth decay and
has a lesser effect on blood glucose. The chemical property of
maltitol is known as 4-O-a-glucopyranosyl-D-sorbitol.
Some researchers have already studied the effects of sugar
alcohol on the physicochemical properties of starch. Lourdin, Bizot,
Colonna, and Coignard (1997) indicated that sorbitol was one of the
natural plasticizers for starch vitreous behavior whereas other researches held that sorbitol, depending on its concentration in
the starch system, behaved as an antiplasticizer (Gaudin,
Lourdin, Forssell, & Colonna, 2000; Mantzari, Raphaelides, &
Exarhopoulos, 2010). The freezing behavior of corn starch gels
with xylitol, mannitol, and sorbitol exhibited higher freezing levels
than that of corresponding sugars (Baek, Yoo, & Lim, 2004; Kim,

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Q. Sun et al. / LWT - Food Science and Technology 62 (2015) 319e324

Yoo, Cornillon, & Lim, 2004). However, few studies have reported
the effect of maltitol on the physicochemical properties of wheat
starch (WS), especially with HMT.
The objective of this research is to study the effect of HMT with
maltitol on pasting properties, thermal properties, morphological
and structural properties of WS. This study will give new ways to
application of sugar-free starchy products.
2. Materials and methods
2.1. Materials
Wheat starch (WS) was supplied by Tianjin Tingfung Starch
Development Co., Ltd (Tianjin, China). Maltitol was purchased from
Futaste Co., Ltd (Shandong, China). All other reagents used were of
analytical grades.
2.2. Methods
2.2.1. Samples preparation
Maltitol was mixed with WS (MAWS) at a solid weight ratio of
0.5:1 based on starch (dry weight), and then modied by HMT
(HMT-MAWS) according to Hoover & Vasanthan, 1994. The content
of moisture of samples was adjusted to 20 g/100 g by adding the
appropriate amounts of distilled water into the containers. The
containers were hermetically sealed and equilibrated at ambient
temperature for 24 h. Resulting samples were then placed in an
electric oven at 100
C for 12 h, dried at 40
C, ground and sieved
(0.15 mm). WS modied by HMT (HMT-WS) was mixed with maltitol at a solid weight ratio of 0.5:1 based on starch (dry weight), the
nal sample maltitol-HMTWS (MA-HMTWS) was then obtained.
2.2.2. Pasting properties
Pasting properties of samples were determined by using RVA-4
(Newport Scientic Pvt. Ltd., Warriewood, Australia) according to
the methods (Singh, Isono, Srichuwong, Noda, & Nishinari, 2008). A
suspension of 3 g (12 g/100 g moisture basis) starch in 25 g of
accurately weighed distilled water underwent a controlled heating
and cooling cycle under constant shear. The slurry was then
manually homogenized by using a plastic paddle to avoid lump
formation before the RVA run. The rotating speed was maintained
at 160 rpm along the process. Parameters including peak viscosity
(PV), viscosity at the end of hold time at 95
C or trough viscosity
(TV), nal viscosity (FV) at the end of cooling, breakdown
(BD PV  TV), setback (SB FV  TV) and pasting temperature
were recorded.

The freeze-dried samples and uncooked granule samples were

nely milled and then placed under vacuum on a double-sided
Scotch tape, mounted on an aluminum specimen holder and
coated with a thin lm of gold. Samples were observed under a Jeol
scanning electron microscope (JSM 840, Jeol, Tokyo, Japan).
2.2.5. X-ray diffraction
X-ray diffractograms of samples were obtained with an X-ray
diffractometer (XRD-6000, Shimadzu, Tokyo, Japan). The scanning
region of the diffraction ranged from 5 to 60
with a target voltage
of 45 KV, current of 40 mA and scan speed of 1
/min.
2.2.6. Statistical analysis
All experiments were conducted at least three times, for which
mean values and standard deviations were determined. Additionally, experimental data were analyzed by using Analysis of Variance
(ANOVA), and expressed as mean values standard deviations.
Differences were considered at signicant level of 95% (p < 0.05).
Pearson's correlation coefcients among other parameters were
calculated by using SPSS 17.0 software.
3. Results and discussion
3.1. Pasting properties
RVA proles of WS, HMT-WS, MAWS, HMT-MAWS and MAHMTWS are presented in Fig. 1 and the corresponding pasting
parameters are summarized in Table 1. The pasting temperature
and setback of HMT-WS increased compared with that of the native
WS. However, its peak viscosity, trough viscosity and breakdown
decreased. In previous works, HMT-modied starches displayed an
increased pasting temperature and a decreased pasting viscosity,
regardless of origin (Hoover & Vasanthan, 1994; Stute, 1992;
Varatharajan,
Hoover,
Liu,
&
Seetharaman,
2010;
Watcharatewinkul, Puttanlek, Rungsardthong, & Uttapap, 2009),
these ndings were consistent with our results. The pasting temperature and breakdown of MAWS slightly decreased, but the peak
viscosity, through viscosity, nal viscosity and setback increased
signicantly. The addition of maltitol formed more hydrogen bonds
with starch and inhibited the movement of starch chains which
strengthened system dynamics, so the viscosity of starch paste
increased. Previous researches showed that when the concentration of sorbitol was low (<60 g/100 g), the addition of sorbitol
reinforced association among the starch chain, polyol and water

2.2.3. Thermal properties

Thermal properties of samples were assessed by a Pyris-1 differential scanning calorimeter (DSC) (PerkineElmer Co., Norwalk,
CT, USA). The instrument was calibrated with indium and an empty
pan was used as reference. Samples were hermetically sealed and
equilibrated at ambient temperature for 24 h. Sample pan was
heated from 25
C to 120
C at 10
C/min. The onset (To), peak (Tp)
and conclusion (Tc) gelatinization temperature as well as enthalpy
(DH) were computed.
2.2.4. Scanning electron microscopy (SEM)
The surface topography of samples was observed with scanning
electron microscopy (SEM) by using the method of Kim et al.
(2008). WS, HTM-WS, MAWS and HTM-MAWS were cooked in
boiling water for 20 min to prepare the gel samples, and then put
into an ultralow temperature freezer and freeze dried for 48 h.
Freeze-drying was carried out in the vacuum chamber where the
chamber pressure was set to 0.13 Pa at room temperature (21
C).

Fig. 1. Pasting properties of WS in the presence of maltitol with heat-moisture

treatment. WS: Wheat starch; HMT-WS: Wheat starch modied by heat-moisture;
MAWS: Mixture of maltitol and wheat starch; HMT-MAWS: Mixture of maltitol and
wheat starch modied by heat-moisture; MA-HMTWS: Mixture of maltitol and heatmoisture treatment modied wheat starch.

Q. Sun et al. / LWT - Food Science and Technology 62 (2015) 319e324

321

Table 1
Pasting parameters of WS in the presence of maltitol with heat-moisture treatment.
Samples

Pasting Temperature(
C)

WS
HMT-WS
MAWS
HMT-MAWS
MA-HMTWS

73.95
75.85
72.85
82.10
76.85

0.07d
0.35c
0.35e
0.71a
0.49b

Peak Viscosity(RVU)
488.39
402.54
502.71
383.42
435.50

1.65b
0.41d
0.59a
1.18e
0.59c

Trough Viscosity(RVU)
322.71
316.63
396.58
333.21
358.42

1.53d
6.78d
4.07a
5.36c
4.71b

Final Viscosity(RVU)
501.32
502.21
584.58
500.08
533.13

1.47c
0.18c
8.13a
5.07c
5.72b

Breakdown(RVU)
165.68
85.92
106.13
50.21
77.08

4.42a
6.36c
2.18b
4.18e
4.12d

Setback(RVU)
178.61
185.58
188.00
166.88
174.71

0.06b
6.95a
2.59a
0.29d
3.43c

WS: Wheat starch; HMT-WS: Wheat starch modied by heat-moisture; MAWS: Mixture of maltitol and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch
modied by heat-moisture; MA-HMTWS: Mixture of maltitol and heat-moisture treatment modied wheat starch.
All data represent the mean of three determinations.
Means with the same letter in each column are not signicantly different (p < 0.05).

thus decreased water mobility in the dispersion and so the viscosity

of starch paste increased (Gaudin et al., 2000; Mantzari et al., 2010).
Compared to MAWS, the pasting temperature of HMT-MAWS
increased from 72.8
C to 82.1
C, but the peak viscosity, through
viscosity, nal viscosity, breakdown and setback decreased by
about 120 RVU, 63 RVU, 84 RVU, 56 RVU and 22 RVU respectively.
The values of pasting viscosity, breakdown and setback were arranged in the order of MAWS > MA-HMTWS > HMT-MAWS. The
results indicated that the interplay between starch chain and polyol
was reinforced during heat-moisture treatment. During pasting,
the swelling of WS was inhibited signicantly by the maltitol with
heat-moisture treatment, so the pasting viscosity decreased and
the pasting temperature increased signicantly. HMT strengthened
the stability of MAWS paste during continued shearing and heating.
3.2. Thermal properties
Fig. 2 shows DSC thermograms of WS, HTM-WS, MAWS and
HTM-MAWS and Table 2 illustrates the onset, peak and conclusion
temperatures of gelatinization (To, Tp, Tc) and the gelatinization
enthalpies (DH). All samples exhibited only a single endothermic
peak. The endothermal transition of HTM-WS and HTM-MAWS
shifted to the higher temperature.
HMT increased the To, Tp, Tc, Tc-To but decreased the DH of WS.
Increases in gelatinization temperatures on heat-moisture treatment have also been observed by other researchers (Adebowale &
Lawal, 2003; Hoover & Vasanthan, 1994). The decrease in DH on
heat-moisture treatment of WS attributed to the disruption of some
of the original double helix.
The addition of maltitol increased the To, Tp, Tc but decreased
DH of WS. Similar results were found in the mixture of starches and
sugars (Maaurf, Che Man, Asbi, Junainah, & Kennedy, 2001;
Thirathumthavorn & Trisuth, 2008). These were due to the

Fig. 2. DSC curves of WS (a), HMT-WS (b), MAWS (c) and HMT-MAWS (d). WS: Wheat
starch; HMT-WS: Wheat starch modied by heat-moisture; MAWS: Mixture of maltitol
and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch modied by
heat-moisture.

formation of hydrogen bonds between maltitol and starch chains.

The amorphous and crystallites region were rearranged and starch
swelling was inhibited by maltitol. The gelatinization temperature
was increased and thermal enthalpy was decreased. Compared to
MAWS, To, Tp, Tc, Tc-To and DH of HMT-MAWS increased signicantly. Some maltitol formed hydrogen bonds with starch in
amorphous and/or crystallites region, and restricted the mobility of
chains, but other free maltitol inhibited the mobility of starch
chains and reduced the availability of water in the system during
HMT, so that higher temperature and thermal enthalpy were
needed to gelatinize starch.

3.3. Analysis of scanning electron microscopy (SEM)

Scanning electron micrographs of WS, HTM-WS, MAWS and
HTM-MAWS before gelatinization are presented in Fig. 3. It showed
that the WS granules had two components: bigger wheat A-type
and smaller wheat B-type granule. Native WS granules had oval and
spherical shapes with smooth surfaces. The surface of modied
starch granules by HMT appeared hollow and irregularly shaped.
The concavities and indentation of the modied starch granules
were evidence of the weak tissue affected by heat-moisture treatment. Similar results were found by other researchers
(Jiranuntakul, Puttanlek, Rungsardthong, Punchaarnon, & Uttapap,
2011; Lin et al., 2010; Vanier et al., 2012; Zavareze, Stork, Castro,
Schirmer, & Dias, 2010). The surface of HTM-MAWS was smooth
and irregular on which a layer of membrane-like substance was
adhered to, but the surface of MAWS was rough with a signicant
quantities of maltitol particles adhered to it. These ndings indicated that maltitol interacted with the starch granules which prevented particles forming as a result of HMT.
After being cooked in boiling water for 20 min and then freezedried, the network of WS, HTM-WS, MAWS and HTM-MAWS were
observed by SEM (presented in Fig. 4). The gure showed that a
spongy structure, and at the same time, a brillar network of WS
gels were formed after the freeze-dry process due to ice crystal
formation. The microstructure of WS gel was characterized by
fragmented structure due to numerous pores. The matrix surrounding the pores was very thin. The pore size of HTM-WS
network was much bigger than that in WS network, and the matrix surrounding the pores was thicker. The heat-moisture treatment decreased the ability of water combining, so there was more
water forming larger ice crystals, leading to bigger holes in network
of HTM-WS.
Compared to the MAWS gel, the pores of HTM-MAWS gel were
smaller and the matrix surrounding the pores was thicker. The gel
net structure of HTM-MAWS was tighter than MAWS. The phenomenon revealed that heat-moisture treatment induced the correlation between maltitol and starch. Similar results regarding
effects of sugars on tapioca starch were reported by Zhang, Tong,
and Ren (2012). They found that the pore sizes of gels containing

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Q. Sun et al. / LWT - Food Science and Technology 62 (2015) 319e324

Table 2
Thermal properties of WS, HMT-WS, MAWS and HMT-MAWS.
Samples

To(
C)

WS
HMT-WS
MAWS
HMT-MAWS

56.55
57.45
61.00
63.85

Tp(
C)
0.07d
0.07c
0.28b
0.21a

61.65
67.45
65.95
69.00

Tc(
C)
0.07d
0.07b
0.64c
0.28a

65.75
72.45
70.05
73.35

DH(J/g)

Tc-To

0.21d
0.21b
0.64c
0.21a

9.20
15.10
9.05
9.50

0.02c
0.10a
0.03d
0.10b

10.15
9.08
9.54
9.74

0.13a
0.20d
0.74c
0.14b

WS: Wheat starch; HMT-WS: Wheat starch modied by heat-moisture; MAWS: Mixture of maltitol and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch
modied by heat-moisture.
All data represent the mean of three determinations.
Means with the same letter in each column are not signicantly different (p < 0.05).

Fig. 3. Scanning electron micrographs of WS, HMT-WS, MAWS and HMT-MAWS. WS: Wheat starch; HMT-WS: Wheat starch modied by heat-moisture; MAWS: Mixture of maltitol
and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch modied by heat-moisture.

trehalose were the smallest and the matrices surrounding them

were the thickest. The starchestarch and/or starchemaltitol interactions were facilitated to form thick matrices due to the high
solid concentration in the amorphous regions and water molecules
coagulated into ice crystals and formed a separate phase. Upon
freeze drying, ice sublimated and left the starch gels in a spongelike state. The sizes of pores and the thickness of the matrices
were correlated with the intermolecular hydrogen bonds between
maltitol and starch molecules.

previous study of HMT starch from wheat, oat (Hoover &

Vasanthan, 1994) and mung bean starch (Li, Ward, & Gao, 2011).
Compared to the native WS and HTM-WS, addition of maltitol
increased the numbers of diffraction peaks. The intensity of
diffraction peaks at 14.6
, 15.3
, 18.7
, 20.6
and 21.8
2q of HTMMAWS were stronger than that of MAWS. The gure also showed
that the area of the amorphous region of HMT-MAWS was
increased than that of MAWS. The phenomenon could be explained
by maltitol particles melted during HMT and then interacted with
starch that could not recrystallize after cooling.

3.4. Analysis of X-ray diffraction (XRD)

4. Conclusion
X-ray diffractograms of WS, HTM-WS, MAWS and HTM-MAWS
were presented in Fig. 5. WS showed the typical A-pattern with
strong peaks at 15
and 23
and a doublet at 17
and 18
2q. Heatmoisture treatment did not change the crystalline pattern. The
relative crystallinity of HTM-WS (29.2%) was higher than the native
starch (27.5%). The reason was that HMT caused associations of new
crystallization with small existing crystalline regions of the starch
granule. The increased X-ray intensity is in agreement with

Physicochemical properties, such as pasting properties, thermal

properties, and structural properties of WS were signicantly
affected by HMT with maltitol. HMT strengthened the interaction
between maltitol and starch. The properties of HMT-MAWS were
affected more remarkably than that of MAWS and MA-HMTWS,
indicating it was more useful to heat-moisture treat the mixture
of maltitol and WS. The results suggested that the interplay

Q. Sun et al. / LWT - Food Science and Technology 62 (2015) 319e324

323

Fig. 4. Scanning electron micrographs of WS, HMT-WS, MAWS and HMT-MAWS gels after freeze drying. WS: Wheat starch; HMT-WS: Wheat starch modied by heat-moisture;
MAWS: Mixture of maltitol and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch modied by heat-moisture.

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Fig. 5. X-ray diffractograms of WS, HMT-WS, MAWS and HMT-MAWS. WS: Wheat
starch; HMT-WS: Wheat starch modied by heat-moisture; MAWS: Mixture of maltitol
and wheat starch; HMT-MAWS: Mixture of maltitol and wheat starch modied by
heat-moisture.

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