Food Chemistry 427 (2023) 136723
2
gelatinization characteristics, crystal structure, long-range and short-
range molecular order degree, water migration, expansion degree and
solubility of wheat starch were systematically measured. Besides, the
microstructure of WOP-WS gel was observed, and we proposed the hy-
pothesis that WOP could inhibit the staling of WS gel by coating starch
particles and reducing starch leaching.
2. Materials and methods
2.1. Materials and preparation of WS-WOP gel
The WS (99% purity, 24.2% amylose content, 62.4% amylopectin
content, 13% moisture, dry basis) was obtained from Shanghai Yuanye
Bio-Technology Co., Ltd. The WOP (food-grade, 90% purity) obtained
from Xi’an BaiChuan Biological Technology Co., Ltd. (Xi’an, China) had
not been further puried. And other reagents were analytical grade.
WS (6%, w/v)-WOP (on the basis of WS, 0, 0.5, 1, 1.5%) gels were
made based on our recent work (Zhou et al., 2022). The mixture solution
was stirred at 30 ◦C for 30 min, then the mixture was heated at 95 ◦C for
30 min.
2.2. Dynamic rheology
The DHR-2 rheometer (TA Instruments, New Castle, DE, USA) was
used to measure dynamic rheological properties. A parallel plate ge-
ometry of 1 mm gap and 40 mm diameter was selected. Scanning was
performed at an angular frequency of 1–100 s
−1
in the linear viscoelastic
region of 1% strain under frequency sweep scanning. The energy storage
modulus (G
′
) and loss modulus (G
″
) of the gels were measured (Xiong, Li,
Shi, & Ye, 2017).
2.3. Pasting properties analysis (RVA)
The viscosity of WS-WOP was studied using rapid viscosity analyzer
(RVA-Super 4, Perten, Sweden). The settings were as follow, 50 ◦C for 1
min, heated to 95 ◦C at a constant rate of 12 ◦C /min and kept for 2.5
min, and then cooled back to 50 ◦C at the same rate and kept for 2 min.
The sample parameters were obtained by RVA software (Ma, Zhu, &
Wang, 2019).
2.4. Hardness test
The texture analyzer (TA.XTC-18, Shanghai Bosin Industrial Devel-
opment Co., Ltd., China) was used to evaluate the hardness property of
WS-WOP gels. The gel was placed under the center of TA/50 probe (Fu
et al., 2021). The setting was: pretest speed 1 mm/s, test speed 3 mm/s,
trigger force 5 g, compression variable 50%, and interval time 5 s. The
experiment was repeated 3 times.
2.5. X-ray diffraction (XRD)
The XRD patterns of lyophilized WS-WOP gel powders were
measured by Cu-K
α
irradiation (λ =1.54056 Å) at 40 kV and 40 mA
currents (XRD, Empyrean, PANalytical B.V, Netherlands). Samples were
scanned at room temperature with a frequency of 4◦/min ranging from 4
to 40◦. The relative crystallinity was analyzed with Jade 6.5 software
(Liu et al., 2020).
2.6. Low-eld nuclear magnetic resonance (LF-NMR)
In order to observe the water migration behavior of WS-WOP gel, LF-
NMR (NMI20-015 V, Niumag Electric Corporation, China) was used
(Xiao et al., 2020). Relaxation curves were obtained using CPMG (Carr-
Purcell-Meiboom-Gill) pulse sequence, and the relaxation time T2 and
the corresponding relative peak areas, as well as area ratios, were
calculated and recorded.
2.7. Solubility and swelling power
Swelling power (SP) and solubility (S) were determined with minor
modications based on previous study (Cui, Fang, Zhou, & Yang, 2014).
After the gel had cooled to room temperature, the 20 g starch gel was
weighed and transferred to a 50 ml centrifuge tube, centrifuged (TGL-
20bR, Shanghai Anting Scientic Instrument Factory, China) at 3000g
for 20 min, and the quantity of the precipitation was weighed in
centrifuge tube. Then the supernatant uid in 105 ◦C oven drying to
constant weight. S and SP were calculated according to Eqs. (1) and (2).
S(%) = [W2/W0] × 100 (1)
SP (g/g) = W1/[W0× (100% −S) ] (2)
W
2
represented the weight of the supernatant after drying (g), W
1
rep-
resented the starch weight on a dry basis (g), W
0
represented the weight
of the precipitate (g).
2.8. Water holding capacity (WHC)
The WS-WOP gel (20 g) was weighed and transferred to the 50 ml
centrifuge tube, then centrifuged at 10,000×g for 10 min, and the pre-
cipitate was weighed after removal of water (Liu, Hong, Gu, Li, & Cheng,
2015). WHC is calculated by the Eq. (3).
WHC (%) = W2/W1×100% (3)
In the formula: W
1
was the weight of gel (g); W
2
was the weight of the
remaining sediment (g).
2.9. Scanning electron microscopy (SEM)
The samples were quick-frozen (BDS3P, Guangdong Bandu Electric
Appliance Co., LTD., China) at −30 ◦C for 1 h and then lyophilized in a
vacuum freeze-dryer at a temperature of −65 ◦C for 72 h. Scanning
electron microscopy (Sigma 300, Zeiss, Germany) was used to take
pictures of the freeze-dried (FD-1A, Beijing Boyiakang Experimental
Instrument Co., Ltd., China) samples (Jia et al., 2022). The magnica-
tion was 500×.
2.10. Fourier-transform infrared spectroscopy (FTIR)
The lyophilized powder was mixed with dried potassium bromide at
a mass ratio of 1:100 and compacted, then placed on a Fourier transform
infrared spectrum sample holder (FTIR, Thermo Nicolet NEXUS670,
Thermo Fisher Science Inc., Waltham, USA). The sample was scanned at
wave numbers ranging of 4000–400 cm
−1
. Each was scanned 25 times
with a resolution of 4 cm
−1
. Omnic and Peakt software were used for
spectral analysis (Su et al., 2020).
2.11. Statistical analysis
The data were statistically analyzed by one-way Analysis of Variance
(ANOVA), and the mean was compared by Duncan’s multiple range test
(P <0.05). SPSS19.0 statistical analysis software was used for statistical
analysis.
3. Results and discussion
3.1. Dynamic rheology
To investigate the rheological properties of WOP-starch gels, G
′
and
G
″
values with different concentrations were detected. G
′
was the
modulus of elasticity, which was used to reect the staling property of
starch gels, in particular short-term amylose staling. G
″
reected the
viscosity modulus of starch gels, as well as its liquid-like property (Jia
L. Wan et al.