foods
Article
The Effect of Different Milling Methods on the
Physicochemical and In Vitro Digestibility of Rice Flour
Yaning Tian 1 , Lan Ding 1 , Yonghui Liu 1 , Li Shi 1 , Tong Wang 1 , Xueqing Wang 1 , Bin Dang 2 , Linglei Li 1 ,
Guoyuan Gou 1 , Guiyun Wu 1 , Fengzhong Wang 3, * and Lili Wang 1, *
Citation: Tian, Y.; Ding, L.; Liu, Y.;
Shi, L.; Wang, T.; Wang, X.; Dang, B.;
Li, L.; Gou, G.; Wu, G.; et al. The
Effect of Different Milling Methods
on the Physicochemical and In Vitro
Digestibility of Rice Flour. Foods 2023,
12, 3099. https://doi.org/10.3390/
foods12163099
Academic Editor: Saroat Rawdkuen
Received: 7 July 2023
Revised: 9 August 2023
Accepted: 11 August 2023
Published: 18 August 2023
Copyright: © 2023 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Foods 2023, 12, 3099. https://doi.org/10.3390/foods12163099
1 Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences, Beijing 100193, China;
jntianyaning@126.com (Y.T.)
2 Tibetan Plateau Key Laboratory of Agric-Product Processing, Qinghai Academy of Agricultural and Forestry
Sciences, Xining 810016, China
3 Key Laboratory of Agro-Products Quality and Safety Control in Storage and Transport Process, Ministry of
Agriculture and Rural Affairs, Beijing 100193, China
* Correspondence: wangfengzhong@caas.cn (F.W.); wanglili03@caas.cn (L.W.)
Abstract: Preparation methods have been found to affect the physical and chemical properties of rice.
This study prepared Guichao rice flour with wet, dry, semi-dry, and jet milling techniques. Differences
in the particle size distribution of rice flour were investigated in order to assess their impact on pasting,
thermal, gel, starch digestibility, and crystalline structure using an X-ray diffractometer (XRD) and a
Rapid Visco Analyzer (RVA) across in vitro digestibility experiments. The results showed that semi-
dry-milled rice flour (SRF) and wet-milled rice flour (WRF) were similar in damaged starch content,
crystalline structure, and gelatinization temperature. However, compared with dry-milled rice flour
(DRF) and jet-milled rice flour (JRF), SRF had less damaged starch, a higher absorption enthalpy
value, and a higher gelatinization temperature. For starch digestibility, the extended glycemic index
(eGI) values of WRF (85.30) and SRF (89.97) were significantly lower than those of DRF (94.47) and
JRF (99.27). In general, the physicochemical properties and starch digestibility of WRF and SRF were
better than those of DRF and JRF. SRF retained the advantages of WRF while avoiding the high
energy consumption, high water consumption, and microbial contamination disadvantages of WRF
and was able to produce better rice flour-associated products.
Keywords: rice flour; milling methods; particle size; physicochemical properties; starch digestibility
1. Introduction
Rice is a basic food on which human beings depend for survival and development.
Rice has a light taste and a high yield and is easy to store, making it popular with merchants
and consumers [1]. About 60% of global people consume rice as their primary food. Rice
contains a high level of carbohydrates and is rich in vitamins and minerals [2]. Since rice is
gluten-free, consuming it is considered one of the most effective ways to treat celiac disease
(CD) [3,4]. In addition to directly cooking and eating rice, it may be processed into puffed
rice and rice flour [5]. Rice flour is extensively processed for various foods, such as bread,
noodles, biscuits, and other gluten-free products. Rice flour is made from rice that has been
milled. Amylose content in indica rice is higher than that in japonica rice, and amylose
molecules age easily and can quickly form into gel, making indica rice more suitable for
making rice flour and rice pasta [6].
During the preparation of rice flour, the milling of raw rice is the most important step,
and milling methods mainly include wet, dry, semi-dry, and jet milling. Soaked samples
can be wet-milled with water and then dried into rice flour [7]. Soaking significantly affects
the qualities of wet-milled rice flour (WRF). For example, soaking reduces the hardness of
rice and helps achieve a finer particle size and delicate texture in WRF, thus increasing the
quality and yield of rice flour products [5,8]. Another commonly used method is the dry
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Foods 2023, 12, 3099 2 of 12

milling method. Dry-milled rice flour (DRF), which is low in moisture content and has a
long storage life, can be produced through direct milling and sieving [8]. However, dry
milling affects the distribution of different particle sizes in rice flour and causes damage
to starch particles, which can lead to changes in the processing properties of rice flour
products [9]. To avoid high levels of damaged starch in dry milling and high energy
consumption, water consumption, nutrient loss, and microbial contamination during wet
milling, semi-dry milling has been used in grain milling [10]. Soaked rice and milling are
semi-dry processing methods, and semi-dry-milled rice flour (SRF) has similar properties
to WRF [11]. Jet milling technology is a new food processing technology that is extensively
applied in the food, cosmetics, medicine, metallurgy, and aerospace fields [4]. Compared
with traditional mechanical processing methods, jet-milled rice flour (JRF) has higher degree
of comminution, certain interfacial activity, an increased specific surface area, reduced
interfacial tension, as well as an improved color, flavor, and texture [12]. Different milling
methods can cause differences in particle size and damaged starch content, which can
affect the processing characteristics of rice-based foods [10]. Wang et al. (2020) concluded
that damaged starch can influence the gelatinization, pasting, and in vitro digestibility of
starch-based foods [13].
Because of the high starch content in rice flour, starch digestibility has a significant
influence on the biochemical indicators of human blood glucose [14]. This may lead to
diet-related health complications like type 2 diabetes [15]. Therefore, the starch digestibility
of rice flour is of increasing interest. The lower degree of hydrolysis can effectively reduce
the rise in blood glucose after meals [16]. Hosson et al. (2015) compared the digestibility
of hammer-milled flour, jet-milled flour, and submicron-scale WRF and suggested that
submicron-scale WRF was more easily digested [17]. Lee et al. (2019) compared hammer
milling and air jet milling, using germinated brown rice as the sample. Coarse fraction
jet-milled flour exhibited higher starch hydrolysis levels [18]. It can be concluded that
milling methods influence the digestibility of rice flour starch by varying the particle size,
damaged starch content, and crystalline structure [16]. Therefore, it is of interest to research
the impact of different four preparations and particle sizes for the in vitro digestion of
rice flour.
Rice flour is the main material used for rice-based foods, and the physicochemical
properties and digestibility of raw materials determine food quality, so it is essential to
study the preparation of raw materials. This study aims to investigate the impact of four
preparation methods on the particle size distribution and its effect on the damaged starch
content, pasting, thermal and gel properties, and starch digestibility of flour. This study
expects to obtain low GI rice flour with better physicochemical properties that can enhance
the quality of rice flour-related products.

2. Materials and Methods

2.1. Materials
Guichao rice (early indica rice) was bought from Jiangxi Huadachang Food Industry
Co., Ltd. (Ganzhou, China) in 2019. The water content was 8.08 g/100 g, the protein content
was 8.36 g/100 g, the lipid content was 0.73 g/100 g, the ash content was 0.77 g/100 g,
the total starch content was 84.04 g/100 g, and the amylose content was 21.61 g/100 g.
The procured rice was kept at −20 ◦ C before experimental use. The porcine pancreas
α-amylase, pepsin, pancreatin, and amyloglucosidase (AMG) were obtained from Sigma-
Aldrich Trading Co., Ltd. (Shanghai, China). The D-Glucose Assay Kit (GOPOD format),
Total Starch Assay Kit, Starch Damage Assay Kit, and Amylose Assay Kit were procured
from Megazyme International Ireland Ltd. (Wicklow, Ireland). The chemicals employed in
this research were of analytical quality.

2.2. Preparation of Rice Flour

WRF: In 4 kg of deionized water, 2 kg of sample was soaked at 25 ◦ C for 6–8 h. The
soaked rice was mixed with 1 kg of distilled water and coarsely milled in a colloid mill (JMS-
Foods 2023, 12, 3099 3 of 12

30A, Langfang Langtong Machinery Co., Ltd., Langfang, China). The coarse pulverized
pulp was then milled for 3 cycles with a gap of 0.10–0.15 mm [19]. Thereafter, the rice pulp
was freeze-dried and passed through standard sieves of 80 mesh and stored in a hermetic
bag at 4 ◦ C until use.
SRF: A total of 2 kg of the sample was mixed with the required amount of water and
soaked at 25 ◦ C. The sample was sealed and shaken, then left to be tempered at 25 ◦ C. The
rice was tempered for 8 h, during which time the rice was shaken every hour to adjust the
moisture content to 27%. The rice was then crushed in a cyclone mill (CT410, FOSS Scino
[Suzhou] Co., Ltd., Suzhou, China) and passed through standard sieves of 80 mesh [19].
The milled rice flour was roasted at 40 ◦ C until water content was below 12%, then kept in
a hermetic bags at 4 ◦ C until needed.
DRF: A total of 5 kg of rice was milled in a cyclone mill (CT410, FOSS Scino (Suzhou)
Co., Ltd., Suzhou, China) and was passed through standard sieves of 80 mesh [20]. The
DRF was stored in a hermetic bag at 4 ◦ C for use.
JRF: A total of 5 kg of rice was milled using an airflow ultrafine mill (Weifang Jinghua
Powder Engineering Equipment Co., Ltd., Weifang, China) and was passed through
200 mesh sieve and were stored in a hermetic bag at 4 ◦ C for use [18].

2.3. Physicochemical Compositions

The contents of moisture, crude protein (GB 5009.5-2016), crude fat (GB 5009.6-2016),
and ash (GB 5009.4-2016) were determined according to the National Standards of China.
The contents of total starch, amylose, and damaged starch were determined using a Total
Starch Assay Kit, Amylose/Amylopectin Kit, and Starch Damage Assay Kit (Megazyme
International Ltd., Wicklow, Ireland), respectively.

2.4. Crystalline Structure of Rice Flour

An X-ray diffractometer (D2 PHASER, Bruker AXS, Karlsruhe, Germany) was used to
determine the crystalline structure of samples. The determination method was carried out
according to the method of Wang et al. (2018) [21]. An appropriate amount of rice flour was
placed in a desiccator (with an internal relative humidity of 100%) and the moisture was
equilibrated for 48 h. The equilibrated rice flour was pressed in the grooves of the glass
sheet so that the sample surface was smooth and level with the glass sheet surface. The
sample was scanned using a Cu–Kα radiation source of 40 kV and 40 mA. The scanning
range was 5–45◦ (2θ), the step width was 0.0131◦ , and the speed was 2◦ /min [16].

2.5. Determination of Particle Size Distribution

A Malvern laser particle size analyzer (Mastersizer 3000, Malvern Instruments, Worces-
tershire, UK) was used to measure the particle size distribution of the dry powder [20].
D10, D50, and D90 were calculated using the software supplied with the device [22].

2.6. Pasting Properties of Rice Flour

The pasting properties of the samples were determined using a Rapid Visco Analyzer
(RVA4500, Perten Instruments, Macquarie, NSW, Australia). Measurements were based
on the method of Gao et al. (2019) [23] with some adaptations. A total of 3.50 g of
sample (14 g/100 g water) was weighed out and distilled water was added to the RVA
jar. The amount of distilled water to be added was identified using the instrument and
corresponded to the moisture content of samples. The determination was made according
to the standard RVA procedure: the samples were maintained at 50 ◦ C for 1 min, warmed
to 95 ◦ C in 198 s, equilibrated at 95 ◦ C for 2.9 min, reduced to 50 ◦ C in 229 s, and then
maintained for 1 min. During this process, Samples were blended with a paddle speed of
960 rpm for 10 s, all other time was 160 rpm [3].
Foods 2023, 12, 3099 4 of 12

2.7. Thermal Properties

A differential scanning calorimeter (DSC-Q200, TA Instruments, New Castle, TL, USA)
was used to determine the thermal properties of a sample. The method of determination
was modeled on the method of Li et al. (2017) [24] with some adaptations. A total of 3 mg
of the sample was added to the crucible, and distilled water 3 times its weight was added.
The samples were sealed and left overnight at 4 ◦ C as blank controls. Determination was
carried out according to the standard DCS-Q200 procedure: the thermal properties curve
was measured by heating from 35 ◦ C to 110 ◦ C at 10 ◦ C/min. The curves were analyzed to
obtain the onset temperature (To), peak temperature (Tp), conclusion temperature (Tc), and
enthalpy change (∆H).

2.8. Gel Properties of Rice Flour

When added to an amount of water, 10 g of rice flour formed a suspension of 15%
mass fraction. The determination method was based on the method of Li et al. (2017) [24].
The mixture was stirred at 35 ◦ C for 1 min and placed in a water bath at 95 ◦ C for 30 min.
The gel was left to cool at 4 ◦ C overnight. The gel properties of the sample were measured
using a texture analyzer (TA-XT 2i/5, Stable Micro System Ltd., Godalming, UK) with a
P/36R probe in texture profile analysis (TPA) mode [4]. The measurement speed of pre-test
and test was 0.5 mm/s. The compression distance was 10.0 mm, the triggering force was
5.0 g, and the compression interval was 3 s [4].

2.9. Determination of Starch Digestibility

The methods of Syahariza et al. (2013) [25] and Zou et al. (2015) [26] with some
modifications were used to determine starch digestibility. This method simulated in vitro
the digestion of starch in the mouth, stomach, and small intestine. A sample equivalent to
50 mg (on a dry basis) of rice starch was added to 2 mL of distilled water and 3 glass beads.
The samples were dispersed and mixed with a vortex oscillator, then boiled in a water
bath for 20 min and cooled. The samples were placed in a 37 ◦ C thermal shaker incubator
(MTH-100, Hangzhou Miu Instrument Co., Ltd., Hangzhou, China) with a 5000 rpm shake
rate. The 1 mL of α-amylase (Sigma A3176) from the porcine pancreas was dropped into
the suspension, and warmed at 37 ◦ C for 2 min. A total of 5 mL of pepsin (Sigma P6887,
pH 2.0) was added and warmed at 37 ◦ C for 30 min. The digest was neutralized by 5 mL
of 0.02 M NaOH, and the pH value was adjusted via 20 mL of sodium acetate buffer. A
total of 5 mg of pancreatin (Sigma P1750) and 43µL of amyloglucosidase (Sigma A7095)
were added to the digesta [16]. The measurement of the glucose concentration was carried
out at specific times, namely 10, 20, 30, 40, 50, 60, 90, 120, 180, and 140 min, and then
dispersed into 1 mL of 95% (v/v) ethanol to terminate the reaction. In addition, 0.1 mL of
glucose (1 mg/mL) was taken as the standard sample, while 0.1 mL of 95% (v/v) ethanol
was used as the blank control. Each analysis was repeated three times. Starch digestibility
was obtained using the following equation:

0.1×1 V × N 162
Dt = A × × × 10 × (1)
As B 180
where A is the absorbance per time point, and As (A sample) is the absorbance of the
standard. V is the volume of the digestive solution, N is the dilution multiple, and B is
the basic dry mass of the sample. The 162 180 expresses the weight coefficient of the starch
(monomeric unit anhydroglucose) converted to glucose [26].
The starch hydrolysis curves were plotted based on the glucose content of samples
sampled at specific time points. The starch hydrolysis rate curves often followed first-order
kinetics, as indicated by Equation (2):
 
Ct = C∞ 1 − e−kt (2)
Foods 2023, 12, 3099 5 of 12

where Ct expresses the glucose concentration at digestive time t, C∞ is the glucose concen-
tration at the final timepoint (240 min), and k is the digestibility coefficient [27].
The area under curve (AUC) was obtained from the k value, as shown in Equation (3):

C∞ h i
AUC = C∞ (t − t0 ) − 1 − exp−k(t−t0 ) (3)
k
The hydrolysis index (HI) is the ratio of the sample AUC to the standard sample
AUC [16], as shown in Equation (4):

AUCsample
HI = × 100% (4)
AUCstandard sample

The calculation of eGI, according to the method of Granfeldt et al. (1992) [28], is shown
in Equation (5):
eGI = 0.862 × H I + 8.198 (5)

2.10. Statistic Analyse

Each sample was duplicated three times and the average value was obtained. All data
were processed using Origin (version 2018, Stat-Ease Inc., Minneapolis, MN, USA) software
and SPSS (version 16.0, SPSS Inc., Chicago, IL, USA).

3. Results and Discussion

3.1. Particle Size Distribution of Rice Flour
The particle size distribution of grain flour affected the physicochemical properties
and processing qualities of sample, which further affected the edibility and sensory quality
of products [29]. The particle size distribution of sample under different methods is shown
in Table 1. As shown, the milling method had a great influence on the particle size. JRF
had a narrow particle size distribution (4.07–29.15 µm) with an average particle size of
14.65 µm, which was significantly smaller than that obtained by other milling methods.
This was due to the full impact of the material driven by the high speed airflow during
jet milling, making the rice flour finer and more uniformly distributed [4]. The average
particle size of WRF was 23.43 µm, of SRF it was 39.10 µm, and of DRF it was 59.45 µm.
Among several milling methods, DRF had the widest particle size distribution (13.30 to
154.50 µm) with more large particles. The average particle size of WRF and SRF were close
to each other, but SRF had a slightly higher average particle size than WRF.

Table 1. Particle size distribution of samples using four milling methods.

Sample DRF SRF WRF JRF

a b c
D10 (µm) 13.30 ± 0.00 9.66 ± 0.47 7.68 ± 0.12 4.07 ± 0.06 d
D50 (µm) 59.45 ± 0.21 a 39.10 ± 0.09 b 23.43 ± 0.09 c 14.65 ± 0.07 d
D90 (µm) 154.50 ± 0.71 a 96.15 ± 4.41 c 107.93 ± 2.52 b 29.15 ± 0.35 d
WRF—wet-milled rice flour; SRF—semi-dry-milled rice flour; DRF—dry-milled rice flour; JRF—jet-milled rice
flour. Values with different letters in the table are significantly different (p < 0.05).

The physicochemical properties and digestibility of sample were largely influenced

by the particle size of rice flour [6]. When comparing the average particle size of the four
types of rice flour, it can be seen that WRF has fine particles, SRF has medium particles,
DRF has coarse particles, and JRF has ultrafine particles. From Figure 1a, it can be seen
that four types of rice flour were irregularly polyhedral-shaped. This is in agreement
with the observations of Farooq et al. [6]. SRF and WRF had smoother surfaces. DRF had
larger particles and rougher surfaces. The ultrafine JRF particles had fewer angles but a
rougher surface.
ds 2023, 12, x FOR PEER REVIEW 6 o

Foods 2023, 12, 3099

particles and rougher surfaces. The ultrafine JRF particles had fewer angles6 but
of 12
a roug
surface.

Figure 1. Scanning electron microscope images of samples (a), damaged starch content (b), X-ray
Figure 1. Scanning electron microscope images of samples (a), damaged starch content (b), X-
diffraction (c), and relative crystallinity of rice flour using four milling methods (d). Values with
diffraction (c),
different andinrelative
letters the figurecrystallinity ofdifferent
are significantly rice flour
(p < using
0.05). four milling methods (d). Values w
different letters in the figure are significantly different (p < 0.05).
3.2. Damaged Starch Content and Relative Crystallinity of Rice Flour
During
3.2. Damaged rice milling,
Starch Content starch
andparticles
Relativecan be damaged of
Crystallinity and even
Rice starch molecular struc-
Flour
ture can be degraded, thus increasing the amount of damaged starch [30]. The main factor
During the
affecting riceprocessing
milling, characteristics
starch particles can
of rice be was
flour damaged
damaged and even
starch starchfollowed
content, molecular str
ture can be degraded,
by particle thus increasing
size distribution the amount
[31]. By comparing of damaged
the effects starch [30].
of four preparation Theon
types main fac
the damage degree of sample (see Figure 1a), evidently, damaged
affecting the processing characteristics of rice flour was damaged starch content, follow starch content varied
significantly among four samples. Among them, WRF had a more granular structure and
by particle size distribution [31]. By comparing the effects of four preparation types on
less damaged starch content, followed by SRF. This indicated that pre-moistening treat-
damage
mentdegree of sample
in the semi-dry milling(see Figure
process 1a), evidently,
effectively reduced thedamageddamaged starchstarch content
content. Onevaried s
nificantly
reasonamong four samples.
for this could be that theAmong them,enough
rice absorbed WRF moisture
had a more to begranular structure
easily milled, thus and l
damaged starch content, followed by SRF. This indicated that pre-moistening
reducing damaged starch content. On the other hand, it could be related to mechanical and treatm
thermal energy [32]. The liquid absorbed the heat generated
in the semi-dry milling process effectively reduced the damaged starch content. during the milling process and One r
reduced the thermal damage to the starch [31]. The dry-milling process generated higher
son for this could be that the rice absorbed enough moisture to be easily milled, thus
mechanical and thermal energy, resulting in more damaged starch content [11]. Although
ducing
the damaged
heat generated starch content.
by material On the
friction in theother hand,
jet-milling it could
process was be related
reduced, theto mechanical
degree of a
thermal energy
damaged [32].
starch The was
content liquid absorbed
the highest. Thisthe
washeatdue to generated
the mechanical during forcethe milling proc
generated
by the high intensity impact that destroyed the starch
and reduced the thermal damage to the starch [31]. The dry-milling process generastructure [18]; thus, the damaged
starch content reached 14.56%. Overall, the mechanical forces and heat in the milling step
higher mechanical and thermal energy, resulting in more damaged starch content [1
significantly influenced the degree of damage to the rice flour.
AlthoughX-ray the diffraction
heat generated
was usedby material
as an analytical friction
methodin the jet-milling
to study the crystalline process
structure wasof reduc
the degree
starch. Fromof damaged
Figure 1b, itstarch content
can be seen wasrice
that four the highest.
flours This peaks
had obvious was due at 15◦to, 17the
◦ , 18mechani
◦,
◦ ◦ ◦
forceand 23 . Among
generated by them,
the highthe connected
intensitydoubleimpact peaks
thatnear 17 and 18
destroyed thewere
starch typical A-type [18]; th
structure
the damaged starch content reached 14.56%. Overall, the mechanical forcesand
starch crystals. It can be inferred that the starch crystalline type was A-type [33,34], and heat
the rice starch crystals remained the same, despite the different methods of milling. This
the milling
indicatedstep that significantly influenced
the crystalline structure of ricethe degree
starch was notof damage
changed by tomechanical
the rice flour.forces
X-ray
and diffraction
different milling was usedThe
methods. assame
an analytical methodbytoMarti
result was obtained study the(2010)
et al. crystalline
[33]. In struct
of starch.
addition,From Figure
it can be seen 1b,that
it can be seen
the peak shapes that
of four
the SRFrice andflours
WRF had obvious peaks
are particularly similar.at 15°, 1
The starch structure of the WRF and SRF was more similar
18°, and 23°. Among them, the connected double peaks near 17° and 18° were typical to that of DRF and JRF.
type starch crystals. It can be inferred that the starch crystalline type was A-type [33,3
and the rice starch crystals remained the same, despite the different methods of milli
This indicated that the crystalline structure of rice starch was not changed by mechani
forces and different milling methods. The same result was obtained by Marti et al. (20
Foods 2023, 12, 3099 7 of 12

The crystallinity degree of rice flour obtained under various milling conditions is pre-
sented in Figure 1c. It was found that the crystallinity degree of rice flour produced under
different milling techniques was similar (p > 0.05). The largest difference in crystallinity
degree was between SRF and JRF, with a difference of 2.45%, while the smallest difference
in crystallinity degree was between DRF and JRF, with a difference of 0.15%. This indicated
that the various flour processing techniques had little influence on the crystallinity of
rice starch.

3.3. Pasting Properties

Rice flour cannot form a gluten network structure, and the main structure of rice flour
products consists mainly of starch gels. Therefore, it is crucial to investigate the effect of
various production processes on the pasting properties of sample, which to some extent
reflected the quality of products [35]. The results are shown in Table 2, the RVA analysis
showed the change in the viscosity of rice flour during heating and cooling. The pasting
temperature was 80.67 ◦ C for WRF and only 72.68 ◦ C for JRF, which was consistent with
the findings of Wu et al. (2019) [4]. This can be associated with damaged starch content.
When damaged starch granules were combined with water, they swelled rapidly and gelled
easily at lower temperatures [22]. Peak viscosity was an important index for measuring
the water-holding capacity of starch [3]. Increased peak viscosity reflected that the starch
granular structure no longer supported swelling and, therefore, that the starch granular
structure was damaged and had begun to deform and break. It can be seen that the peak
viscosity of samples was negatively related to damaged starch. Compared to SRF and WRF,
DRF and JRF had high damaged starch content and low peak viscosity (p < 0.05). The starch
molecules were heated and gelatinized to form a viscous gel [36]. On cooling to 50 ◦ C,
the final viscosity of rice flours began to increase after cooling, indicating the formation
of a rigid gel structure upon cooling. Residual starch granules interacted with leached
molecules and formed a network structure, contributing to the increase in viscosity during
cooling [37]. JRF had the lowest breakdown viscosity, which meant that the gel it formed
was more able to withstand heating and shearing [3]. Interestingly, the peak and final
viscosities of WRF and SRF were significantly higher than those of DRF and JRF (p < 0.05),
suggesting that the water-holding capacity and network structure of these two flours were
improved [8,10]. The setback value can be used to measure the degree of starch aging
and regeneration. WRF and DRF had the highest regeneration values, followed by SRF;
however, all were significantly higher than JRF. This suggested that they have a stronger
gelling ability than JRF [4].

Table 2. Pasting and thermal properties of samples under four milling methods.

Sample DRF SRF WRF JRF

Pasting Properties
Pasting Temperature (◦ C) 73.50 ± 0.05 c 77.12 ± 0.94 b 80.67 ± 0.06 a 72.68 ± 1.17 c
Peak Viscosity (cP) 5466 ± 60 b 5667 ± 25 a 5613 ± 137 a 4960 ± 23 c
Though Viscosity (cP) 3443 ± 100 c 3881 ± 102 a 3822 ± 117 a 3581 ± 49 b
Final Viscosity (cP) 6705 ± 47 c 6863 ± 61 b 7100 ± 106 a 6118 ± 7 d
Breakdown (cP) 2023 ± 43 a 1786 ± 88 b 1790 ± 34 b 1379 ± 25 c
Setback (cP) 3262 ± 60 a 2982 ± 48 b 3278 ± 23 a 2536 ± 56 c
Thermal Properties
To (◦ C) 61.32 ± 0.09 b 60.75 ± 0.12 c 59.29 ± 0.27 c 64.14 ± 0.06 a
Tp (◦ C) 67.07 ± 0.17 b 66.02 ± 0.09 c 64.68 ± 0.13 d 69.54 ± 0.00 a
Tc (◦ C) 71.46 ± 0.51 b 70.14 ± 0.24 c 69.09 ± 0.20 c 74.69 ± 0.08 a
c (J/g) 5.75 ± 0.07 c 7.85 ± 0.13 b 8.21 ± 0.06 a 4.12 ± 0.10 d
To: onset temperature; Tp: peak temperature; Tc: conclusion temperature; ∆H: enthalpy change. Values with
different letters in the table are significantly different (p < 0.05).
Foods 2023, 12, 3099 8 of 12

3.4. Thermal Properties

When a phase change of the material occurs, it is always accompanied by energy
absorption or release. In the DSC analysis, the crystalline structure of starch absorbs heat
during the melting process, which appears as a heat absorption peak. The larger the peak
area, the more heat is required to melt the crystal and the higher the melting enthalpy
change. As shown in Table 2, the milling method had a great influence on the thermal
properties. The DSC results indicated that the gelatinization of rice starch occurred at
a temperature range of 64.68 to 69.54 ◦ C. To, Tp, and Tc in DRF were obviously larger
than in SRF and WRF, which suggests that rice flour with particles of large size can not
easily be pasted [10]. When the temperature reached the onset temperature of rice flour
pasting, small particles combined with water to start gelatinization, while large particles
were not able to react as quickly, so the gelatinization temperature was higher than in
flour with small particles [5]. The damaged starch and particle size in SRF were closer to
those in WRF, so there was no significant difference in To and Tc between SRF and WRF.
Interestingly, the JRF had the smallest median particle size, but the highest To, Tp, and Tc.
The analysis of the data in Table 2 shows that To, Tp, and Tc were positively correlated
with damaged starch content. Compared to the other three milling methods, JRF had the
highest damaged starch content with significantly higher To, Tp, and Tc values (p < 0.05).
However, one study found that samples with smaller particle sizes and more broken starch
had lower Tp and Tc values [38]. This could be due to the effect of non-starch ingredients
(e.g., lipids and protein) on the thermal properties of the flour, such as the denaturation of
protein and the interaction of starch with fat or protein [38,39]. In addition, in samples with
more damaged starch, the aggregation of starch granules affected the starch–water system
formation and gelatinization temperature [40]. ∆H reflects the energy of the transition from
a crystalline to a non-crystalline structure [6]. There was a significant difference in the
∆H of rice flour between the various milling techniques (p < 0.05). The different milling
methods resulted in large differences in damaged starch content. WRF had a maximum ∆H
because WRF had less damaged starch and relatively intact granules, thus requiring more
energy to break the granule structure and absorbing more heat in the process [4]. The ∆H
was negatively correlated with damaged starch content, so JRF had the lowest ∆H value of
the four samples. In general, the thermal properties of the four samples were associated
with changes in particle size and damaged starch content due to preparation methods [38].

3.5. Gel Properties

The texture of products was influenced by the gel properties of the samples. TPA
results are shown in Table 3. DRF and WRF were significantly different in all indicators
(p < 0.05). Compared to WRF, SRF, DRF, and JRF showed increased resilience, springiness,
and chewiness. In terms of hardness, DRF had the highest hardness of 6.96 N, followed by
SRF and, finally, WRF and JRF. The gel hardness of WRF was close to that of JRF (p > 0.05).
In terms of the adhesiveness index, the viscosity of the other three flours was higher than
that of WRF. DRF had the highest hardness, and this was attributed to damaged starch
content. Rice flour was easy to setback when broken starch was high. The setback was due
to increased adhesiveness caused by the rearrangement of amylose during cooling [41].
High DRF setback values indicated a high degree of recrystallisation and an increase in
gel hardness [42,43]. Although JRF had high damaged starch content, its setback values,
adhesiveness, and hardness were different from those of DRF. Qiu et al. (2019) concluded
that the milling method could change the amylose content in samples [44]. The authors of
some studies suggested that this could be due to the non-starch components of rice flour,
and starch and lipids formed starch–lipid complexes [40]. Some studies have shown that
lipids inhibited starch granule swelling and reduced granule setback value and hardness
when gelling [40,45]. In addition, samples with high damaged starch content had poorer
gel properties after pasting, and damaged starch content in the sample should be kept at a
low level to ensure the gel properties of rice products [46].
Foods 2023, 12, 3099 9 of 12

Table 3. Gel properties of samples under four milling methods.

Sample DRF SRF WRF JRF

6.96 ± 0.42 a b 3.50 ± 0.15 c 3.74 ± 0.07 c
Hardness (N) 5.37 ± 0.20
Adhesiveness(N.s) −17.38 ± 3.39 c −14.40 ± 2.23 bc −5.65 ± 0.64 a −11.87 ± 1.25 b
Resilience (%) 4.21 ± 0.82 b 5.48 ± 0.49 a 2.49 ± 0.68 c 4.08 ± 0.75 b
Cohesiveness 0.54 ± 0.03 b 0.52 ± 0.01 b 0.42 ± 0.03 c 0.58 ± 0.01 a
Springiness (%) 94.96 ± 6.18 a 87.76 ± 6.40 b 84.48 ± 8.38 b 96.03 ± 2.92 a
Gumminess 384.01 ± 41 a 286.04 ± 8 b 150.31 ± 15 d 220.81 ± 6 c
Chewiness 362.38 ± 37 a 250.86 ± 16 b 127.93 ± 26 c 212.14 ± 11 b
Values with different letters in the table are significantly different (p < 0.05).

3.6. Starch Digestibility

Many kinds of cereals were crushed before production and processing. The degree
of milling and the size of the flour not only affected the processing properties, such as
water absorption and solubility, but also affected the digestibility of the rice flour products.
Figure 2 shows that the milling method had a significant influence on the starch hydrolysis
of rice flour. JRF exhibited the highest hydrolysis degree (90.59%), followed by DRF
(87.20%), SRF (85.10%), and WRF (83.78%). This phenomenon could be related to particle
size and damaged starch content. In JRF, the particle size was the smallest and damaged
starch content was the highest. This increased the surface area of the particles and made it
easier to contact and react with digestive enzymes, thus increasing the amount of hydrolysis
products [16,18]. Table 4 shows the in vitro starch hydrolysis indexes of rice flour under
different milling techniques. The analysis of data revealed that JRF had the highest K,
C∞, AUC, and eGI values, followed by DRF, SRF, and WRF. Starch hydrolysis indexed
with the increase in damaged starch content. [46]. Different milling methods affected the
surface area, gaps, and cracks of the rice flour particles, thus affecting the digestibility of
rice flour [47]. More damaged starch content and larger gaps allowed for more contact area
between digestive enzymes and particles. The gaps were more convenient for digestive
enzymes to enter into cells for the reaction, causing the rice flour particles to be more
thoroughly digested. As a result, the value of various digestive indexes was higher. JRF
had smaller particles and the highest damaged starch content, resulting in higher water
diffusion and a larger surface area for contact with digestive enzymes [48]. Therefore, the
four indexes of starch hydrolysis were significantly higher than those of the other rice
flour samples. In addition, different milling methods may result in differences in amylose,
amylopectin content, and differences in non-starch components, such as lipids. All these
could affect the digestibility of samples [6,16,18,49]. It is noteworthy that the eGI of SRF and
WRF was significantly lower than that of DRF and JRF (p < 0.05). This may be due to the
semi-dry milling method and the wet milling method retaining more intact cell walls in the
rice flour. The cell walls reduced the contact area for digestive enzymes and increased the
barrier to enzyme entry into the cell [6]. The action area of digestive enzymes on rice flour
particles was reduced and, thus, the eGI of the samples was lower. Low eGI can effectively
control blood glucose and provides health benefits. Generally, the eGI of rice flour products
is higher than that of other cereals, and reducing the eGI of rice flour products is a major
challenge in production [49]. The results of in vitro digestion experiments suggest that it is
feasible to reduce the eGI of samples using the four milling methods.
023, 12, x FOR PEER REVIEW

Foods 2023, 12, 3099 10 of 12

Figure 2. Hydrolysis curves of samples under four milling methods.

Figure 2. Hydrolysis curves of samples under four milling methods.
Table 4. Digestibility of samples under four milling methods.

Table 4. Digestibility
Sample of samples
DRF under four
SRF milling methods.
WRF JRF
K (×10−2 ) 2.99 ± 0.04 b 2.54 ± 0.15 c
2.08 ± 0.01 d 3.32 ± 0.05 a
SampleC∞ (%) DRF
87.20 ± 0.61 b SRF 83.78 ± 0.38
85.10 ± 0.92 c d
WRF90.59 ± 0.66 a
c 189.62 ± 1.12 a
AUC 180.15 ± 1.65b b 170.75 ± 1.28 161.00 ± 0.93 d
K (×10−2)eGI 2.99 ± 0.04
94.47 ± 0.79 b 89.972.54
± 0.61±c 0.15 85.30 ± 0.45 d2.08 ±
c 0.01
99.27
d
± 0.59 a 3.32
C∞ (%) 87.20 ± 0.61 85.10 ± 0.92 83.78 ± 0.38
b significantly different (p < 0.05).
Values with different letters in the table are c d 90.5
AUC
4. Conclusions180.15 ± 1.65
b 170.75 ± 1.28 c 161.00 ± 0.93 d 189.6
eGIThis research
94.47 ± 0.79
compared
b 89.97
the effects of dry, ± 0.61
semi-dry,
c 85.30 methods
wet, and jet milling ± 0.45 don the 99.2
particle
Values withsize, physicochemical
different letters inproperties,
the tableand
aredigestibility
significantlyof rice flour. The(p
different results indicate
< 0.05).
that milling methods had no effect on the crystalline structure of samples. Compared
with DRF and JRF, SRF was close to WRF in terms of damaged starch content, crystalline
4. Conclusions
structure, and gelatinization temperature and had a better network structure. DRF had high
degree of recrystallisation and the highest gel hardness. In terms of rice flour digestibility,
This research compared the effects of dry, semi-dry, wet, and jet milling
the eGI of SRF was significantly lower than that of DRF and JRF, which was close to
the particle size,
that of WRF. physicochemical
In general, WRF and SRF had properties, and digestibility
better physicochemical properties andofstarch
rice flour.
digestibility. Due to the high energy consumption and water consumption
indicate that milling methods had no effect on the crystalline structure of WRF, SRF is of sam
more suitable for the preparation of low-eGI processed rice flour products. In future studies,
paredsemi-dry
with DRF
milledand JRF,will
rice flour SRF wastoclose
be used preparetovarious
WRFtypes
in terms of damaged
of rice flour starch co
products with
talline structure,
a lower glycemic and gelatinization
index, temperature
such as rice noodles andand
and rice cakes, had a better
to assess theirnetwork
starch str
digestibility in vivo and in vitro.
had high degree of recrystallisation and the highest gel hardness. In terms
digestibility, the eGI Conceptualization,
Author Contributions: of SRF was significantly
Y.T.; methodology,lower than that
L.D.; software, of DRF
L.D. and and JRF
L.L.; vali-
dation, L.S. and G.G.; investigation, T.W. and G.W.; resources, Y.L. and B.D.; data curation, Y.T.;
closewriting—original
to that of WRF. In general, WRF and SRF had better physicochemical pro
draft preparation, Y.T.; writing—review and editing, X.W.; visualization, Y.L.;
starch digestibility.
supervision, Due
L.W.; project to the high
administration, energy
F.W. and L.W.consumption and
All authors have read andwater consumpt
agreed to the
published version of the manuscript.
SRF is more suitable for the preparation of low-eGI processed rice flour produc
Funding:
studies, This research
semi-dry was supported
milled by the National
rice flour will be Keyused
Research
toand Development
prepare Program of
various China of rice
types
(2022YFF1100500), the National Key Research and Development Program of China (2016YFD04002), and
ucts with
the Keya lowerandglycemic
Research Developmentindex,
Programsuch asProvince
of Shanxi rice noodles and rice cakes, and to
(202102140601014).
starch digestibility
Institutional Review in vivo
Board and in
Statement: Notvitro.
applicable.

Author Contributions: Conceptualization, Y.T.; methodology, L.D.; software, L.D. and

tion, L.S. and G.G.; investigation, T.W. and G.W.; resources, Y.L. and B.D.; data curatio
Foods 2023, 12, 3099 11 of 12

Informed Consent Statement: Not applicable.

Data Availability Statement: Research data are not shared.
Acknowledgments: All authors wish to thank Yonghu Zhang of the Yuhuang Grain and Oil Food
Co., Ltd., for providing the rice samples.
Conflicts of Interest: The authors declare no conflict of interest.

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