Critical Reviews in Food Science and Nutrition

ISSN: 1040-8398 (Print) 1549-7852 (Online) Journal homepage: https://www.tandfonline.com/loi/bfsn20

Starch modification through environmentally

friendly alternatives: a review

Bianca C. Maniglia, Nanci Castanha, Patricia Le-Bail, Alain Le-Bail & Pedro E.
D. Augusto

To cite this article: Bianca C. Maniglia, Nanci Castanha, Patricia Le-Bail, Alain Le-Bail & Pedro
E. D. Augusto (2020): Starch modification through environmentally friendly alternatives: a review,
Critical Reviews in Food Science and Nutrition, DOI: 10.1080/10408398.2020.1778633

To link to this article: https://doi.org/10.1080/10408398.2020.1778633

Published online: 17 Jun 2020.

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CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION
https://doi.org/10.1080/10408398.2020.1778633

REVIEW

Starch modification through environmentally friendly alternatives: a review

Bianca C. Manigliaa,b,c,d , Nanci Castanhad , Patricia Le-Bailb,c , Alain Le-Baila,c , and Pedro E. D.
Augustod,e
a
ONIRIS-GEPEA UMR CNRS, Nantes, France; bBIA-INRA UR, Nantes, France; cSFR IBSM INRA CNRS, Nantes, France; dDepartment of Agri-food
Industry, Food and Nutrition (LAN), Luiz de Queiroz, College of Agriculture (ESALQ), University of S~ao Paulo (USP), Piracicaba, SP, Brazil;
e
Food and Nutrition Research Center (NAPAN), University of S~ao Paulo (USP), S~ao Paulo, SP, Brazil

ABSTRACT KEYWORDS
Starch is a versatile and a widely used ingredient, with applications in many industries including Starch modification; dry
adhesive and binding, paper making, corrugating, construction, paints and coatings, chemical, heating treatment – DHT;
pharmaceutical, textiles, oilfield, food and feed. However, native starches present limited applica- heat moisture treatment –
HMT; pulsed electric field –
tions, which impairs their industrial use. Consequently, starch is commonly modified to achieve PEF; ultrasound – US; ozone
desired properties. Chemical treatments are the most exploited to bring new functionalities to
starch. However, those treatments can be harmful to the environment and can also bring risks to
the human health, limiting their applications. In this scenario, there is a search for techniques that
are both environmentally friendly and efficient, bringing new desired functionalities to starches.
Therefore, this review presents an up-to-date overview of the available literature data regarding
the use of environmentally friendly treatments for starch modification. Among them, we high-
lighted an innovative chemical treatment (ozone) and different physical treatments, as the modern
pulsed electric field (PEF), the emerging ultrasound (US) technology, and two other treatments
based on heating (dry heating treatment – DHT, and heat moisture treatment – HMT). It was
observed that these environmentally friendly technologies have potential to be used for starch
modification, since they create materials with desirable functionalities with the advantage of being
categorized as clean label ingredients.

Introduction Several characteristics can be changed by the modification

Starch is a carbohydrate formed mainly by two different glu-
cose polymers: amylose and amylopectin (Li et al. 2018).
Highly available in nature, this biodegradable and nontoxic
biopolymer can form consistent pastes and gels when heated
in the presence of a sufficient amount of water.
Consequently, starch is widely used in large quantities as an
industrial ingredient, with broad applications in different
sectors, such as food, feed, paper, textile, laundry finishing,
chemical, petrochemical, pharmaceutical, bioethanol, build-
ing materials and biodegradable products industries (Vanier
et al. 2017).
Unfortunately, starches present limited functionalities in
their native form, which can hinder their applications. Each
starch source presents distinct and characteristic properties,
such as the temperature of gelatinization, the amount of
water absorbed according to the temperature level, the past-
ing capacity and the gel strength, among others. Given that
the economical available sources are highly limited, the pro-
duction of modified starches, therefore, is an alternative that
has been extensively applied in order to improve those prop-
erties and to overcome one or more limitations of the native
starches, increasing their industrial applications.
processes, such as the gelatinization, swelling, solubility,
pasting and retrogradation properties, among others
(Tharanathan 2003). These new ingredients can be applied
in different processes and products, with more desirable
properties when compared to their native form.
For this purpose, different methods (chemical, physical,
enzymatic, and genetic) can be used to obtain starches with
required properties for each industrial application.
The chemical modification methods are the most indus-
trially applied, due to their low cost and easiness of applica-
tion. The most commonly used chemical processes usually
affects the three available hydroxyl groups (at position: C2,
C3 and C6) of the starch molecules, which can be modified
through esterification, etherification and/or oxidation
(Masina et al. 2017). Besides, the glycosidic bonds of the
starch molecules can be depolymerized after chem-
ical treatments.
The traditional chemical modification methods (such as
using hypochlorite, acetates, phosphates, and acids) generate
a large volume of effluents that must be recycled. Due to
their nature, these effluents can be harmful to the environ-
ment. Moreover, the possibility of trace elements in the final
product can limit some applications for these modified

CONTACT Bianca C. maniglia biancamaniglia@gmail.com ONIRIS-GEPEA UMR CNRS, Nantes, France;; Pedro E. D. Augusto pedro.ed.augusto@usp.br
Department of Agri-food Industry, Food and Nutrition (LAN), Luiz de Queiroz, College of Agriculture (ESALQ), University of S~ao Paulo (USP), Piracicaba, SP, Brazil.
ß 2020 Taylor & Francis Group, LLC
2 B. C. MANIGLIA ET AL.
starches, in special in pharmaceutical and food industries
(whose demand for “clean label” ingredients is grow-
ing fast).
Consequently, different alternatives are being developed
to overcome those limitations.
In this review, some “clean” or “green” alternatives for
starch modification are explored, including the most import-
ant thermal and non-thermal physical treatments, as well as
a particular chemical one (ozone). The principles, main
characteristics, and possible applications of each one
are discussed.
Environmentally friendly treatments
Within the last decade, there has been an increasing interest
among researchers to develop “green” methods for starch
modification. In other words, processes with lower environ-
mental impact. Therefore, all the processes here described,
despite being physical or chemical, can be categorized
according to one common characteristic: the claim of being
“clean” technologies, in special when compared with the
traditional chemical methods.
Considering the extensive amount of modification meth-
ods available in the literature, promising modification alter-
natives were selected, based on their academic and industrial
relevance, as described below.
It is important to mention that in the context of this
review, the environmentally friendly treatments are those
that leave no residues in the product or in the environment.
They can be either physical or chemical, both thermal and
non-thermal, and they can be carried out on the presence or
absence of water/moisture. Their main characteristics and
results, explored throughout the literature, are summarized
in this section.
Therefore:

HMT – illustrates a thermal treatment in the presence
of moisture

DHT – illustrates a thermal treatment in the absence
of moisture

PEF – illustrates a non-thermal treatment using pulsed
electric fields

US – illustrates a non-thermal treatment using high
power acoustic fields

Ozone – illustrates a chemical treatment
In fact, the physically modified starches do not need to
be identified on food labels as “modified starches”, making
them attractive for food companies (Bemiller 2018). Due to
their “clean” appeal, different physical modification treat-
ments have been developed. They can be divided in thermal
(dry heating treatment – DHT, and heat moisture treatment
– HMT) and non-thermal (pulsed electric field – PEF, and
ultrasound – US) processes.
Although being a chemical process, ozone is considered a
clean technology by many researchers (Pandiselvam et al.
2019; Klein et al. 2014; Çatal and Ibanoǧlu 2014) – although
different regulatory requirements may apply, depending on
the country and application. Even so, due to its environ-
mentally friendly characteristics, the use of ozone technology
to modify starch was explored in this review.
Physical modification: thermal treatments
Thermal or heat treatments were first reported by Mangels
(1934) as a method of beneficially altering the properties of
flours. Patents detailing industrial processes appeared in the
1960s (Russo and Doe 1970). Even today, thermal treat-
ments are still important from both academic and industrial
perspectives, as can be verified by very recent articles - such
as Bharti, Singh, and Saxena (2019) and Maniglia
et al. (2020).
Purhagen, Sj€oo€, and Eliasson (2012) affirmed that thermal
treatment can be used as a tool to extend the shelf-life of
flours. These authors associated this behavior to the reduc-
tion of moisture content in the lipid-rich fractions and to
the reduction of the enzymatic activity. Heating processes
can also result in significant impact on the starch techno-
functional properties, achieving modifications in their phys-
ical properties. Thermal processes are used for both flours
and starches, therefore, both products are discussed here.
Two basic methods can be distinguished based on the
presence or absence of moisture: dry heating treatment
(DHT) and heat moisture, or hydrothermal treatment
(HMT) (Lehtinen et al. 2003).
Thermal treatments in the presence of moisture: heat
moisture treatment (HMT)
In the heat moisture treatment (HMT) method, the native
starch is subjected to heating in a sealed container with lim-
ited amount of water (usually <35% w/w) at a temperature
above the gelatinization temperature but below the glass
transition temperature, in order to preserve the granular
structure of the starch (Ashogbon 2018). The processing
temperature usually ranges from 80 to 140  C, and the proc-
essing time varies from 1 to 24 h in most processes
(Bemiller and Huber 2015).
The conditions of the HMT can promote significant
changes on starch functionality, affecting some starch prop-
erties as: amount of amylose-lipid complexes, granule
morphology, granule crystallinity, gelatinization and pasting,
gel properties and digestibility, double helix content, swel-
ling power and solubility (Jacobs and Delcour 1998).
Some papers found in literature about the HMT applied
in different starch or flour sources are summarized in Table
1. In general, the physical properties of the treated starch
depend on the botanical source and treatment conditions.
Pinto et al. (2012) treated pinion starch by HMT, obtain-
ing greater thermal stability, which probably enables the use
of HMT pinion starches in canned food industry. The
authors also mentioned that treated pinion starches showed
lower swelling power and solubility than native starch.
These characteristics are desired for use in noo-
dle production.

Table 1. Heat moisture treatment (HMT) applied in different starch or flour sources.
Raw material
Pinion starch
Waxy, rice, corn, and
potato starches
Rice starch and flour
Cassava starch
Arrowroot starch
Elephant foot yam starch
Amaranth starch
Pre-gelatinized maize
starch
Oat starch
Corn, tapioca and
potato starches
Mango kernel starches
HMT: Heat moisture treatment, DH: gelatinization enthalpy; AFM: atomic force microscopy.
Conditions
15, 20 and 25% moisture contents at
100, 110 and 120  C for 1 h
25% moisture content at 100  C
for 16 h
20, 25 and 30% moisture content at
100  C for 16 h
10, 20, and 30% moisture content at
120  C for 60 min
28% moisture content at 100  C for
2, 4, 8, and 16 h
15%, 20%, 25%, 30%, and 35%
moisture content and kept at 4  C/
24 h. Then heated in hot air oven
at 110  C for 3 h
28% moisture content and heated at
110  C for 2.5 h
40% moisture content at 100  C for
3, 12 and 24 h in an air-
drying oven
30% moisture content at 100  C/12 h
30% moisture content and heated at
95–96  C for 0, 30 or 60 min, then
cooled in a 50  C water bath for
30 min heating-holding-cooling
steps: 1–6 iterations
20, 25 and 30% moisture content
and kept at 4  C/24 h. Then heated
in hot air oven at110  C for 3 h
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 3
Major findings Reference
HMT increased the X-ray peaks intensity and gel hardness and Pinto et al. (2012)
reduced its relative crystallinity of pinion starch. HMT
reduced the solubility, swelling power, peak viscosity,
breakdown, and DH of the pinion starch. HMT increased the
pasting temperature, final viscosity, setback and the
gelatinization temperatures of the pinion starch. The
modification of starch properties was more pronounced as
the moisture used in the process increased.
HMT promoted changes in the surface structure of starch Jiranuntakul
granules (AFM images), creating smoother surface, mainly in et al. (2013)
the case of normal rice, waxy rice, corn starches. Treated
starches showed starch granule architecture of the type
block model. Finally, HMT caused a reduction in the size of
the protrusions on the surface of the potato starch granules.
Increase of moisture content in the HMT resulted in rice starch Puncha-Arnon and
and flour with higher pasting temperature, lower peak Uttapap (2013)
viscosity, and gels with lower hardness. Increase of moisture
content in the HMT resulted in rice starch and flour with
higher gelatinization temperature. HMT with 30% moisture
content resulted in rice starch with lower DH and rice flour
with higher DH. HMT had a far greater effect on the flour
than starch properties.
The treated starches showed lower DH, higher peak Andrade, De
temperature and pasting temperature and lower viscosity Oliveira, Colman,
peak in relation to the native starch; The HMT not affected Da Costa, and
the average diameter of the starch granules (observed by Schnitzler (2014)
the AFM technique), however this treatment promoted a
reduction in the relative crystallinity. The changes were
greater as the moisture content of the HMT increased. In
addition, the treated starches showed a slight tendency to
yellow color.
HMT promoted change in the crystallinity pattern of arrowroot Pepe et al. (2016)
starch (native: CA-type and treated: A-type). Treated
starches showed higher pasting temperature and lower
peak viscosity, higher gelatinization temperature and
crystallinity, and lower DH, swelling power, and solubility
than the native one. Modified starches resulted in gels more
stable and stronger, with higher storage and loss modulus,
resistance to shearing and heat than gels from native
starch. It was concluded that 4 h of HMT was enough to
promote significant changes in the physicochemical
properties of starch.
HMT resulted in starch with granular aggregation, fissures and Sukhija, Singh, and
cavities on the granule surfaces, reduction in the Riar (2016)
crystallinity, color, and water activity but there was no
alteration in the crystalline structure (C-type). The solubility,
gelatinization temperature, pasting temperature were higher
but swelling power and the DH were lower in treated
starch than the native one.
Amaranth starches treated resulted in noodles with lower Chandla, Saxena,
cooking loss, firmer texture, better taste and aroma in and Singh (2017)
comparison to the control noodles.
HMT time affected positively in the ‘slowly digestible starch’ Agama-Acevedo
and in the resistant starch content. HMT affected in the et al. (2018)
crystallinity pattern of maize starch.
HMT promoted reduction of the amylose content, swelling Kaur and
power, solubility and altered the crystallinity pattern (B and Singh (2019)
type starch granules proportion). Treated starches showed
lower paste clarity, peak and breakdown viscosities than the
native. However, HMT not affected the shape of oat starch.
The DH changes and the swelling power reduced for all Lin, Lin, Lin, and
treated starches (effect quantity: corn < tapioca < potato). Chang (2019)
The properties of starch have been more altered as iteration
number and holding time.
HMT not affected the amylose content, but increased the Bharti, Singh, and
water and oil binding capacities, reduced the swelling Saxena (2019)
power and relative crystallinities, and increased solubility of
the treated starch when compared with native. HMT
starches showed higher pasting temperature, peak viscosity,
setback and final viscosity, and dents and pits on the
granules surface.
4 B. C. MANIGLIA ET AL.
Jiranuntakul et al. (2013) investigated changes on the sur-
face of corn, potato, waxy and normal rice starch granules
after HMT using atomic force microscopy (AFM). The
authors observed alteration in the granule morphology with
the HMT (development of small protrusions, smooth areas,
and round-shaped depressions). The authors also observed
that the new surface of starch treated by HMT showed
greater capacity to block the penetration of water into the
starch granules.
Puncha-Arnon and Uttapap (2013) investigated the HMT
effect in the properties of the rice starch and flour. They
observed that HMT had a greater effect on the properties
(pasting viscosity, gelatinization and gel hardness) of the
flour than of the starch. The authors associated this behavior
with the presence of proteins in flour.
Andrade et al. (2014) studied the effect of HMT in
organic cassava starch. Rheological properties such as the
pasting temperature and the peak temperature increased,
while gelatinization enthalpy decreased. The HMT not
affected in the average diameters of the granules, however
reduced the degree of relative crystallinity of the cas-
sava starch.
Pepe et al. (2016) investigated the effect of HMT on
structural, rheological, and physicochemical characteristics
of arrowroot starch. Pastes from modified starches showed
reduction of pseudoplasticity. Compared to the native
starch, the treated starches showed more organized chains,
greater paste stability and stronger gels, with greater resist-
ance to shear and heat even after of extreme situations, such
as acid or sterilization conditions.
Sukhija, Singh, and Riar (2016) investigated the effect of
HMT in the morphological, physicochemical, and functional
properties of elephant foot yam starch. The results of this
study showed that HMT significantly altered these proper-
ties, but it did not alter the crystalline structure type
of granules.
Chandla, Saxena, and Singh (2017) evaluated the amar-
anth starch treated by HMT for development of noodles.
The work showed that HMT improved the amaranth starch
properties to be used for noodles production, because this
treated starch resulted in noodles with better texture and
eating attributes.
Agama-Acevedo et al. (2018) evaluated the effect of HMT
on resistant starch content of pregelatinized high-amylose
maize starch. HMT had an important effect on the freeze-
dried sample as demonstrated by the increase in the content
of ‘slowly digestible starch’ and in the content of resist-
ant starch.
Kaur and Singh (2019) studied the HMT effect on physi-
cochemical and functional properties of starches from eight
Indian oat cultivars. Treated starches showed lower solubil-
ity, lower apparent amylose content, different particle size
distribution with lower proportion of B-type (5–16 lm) and
C-type (<5 lm) starch granules, lower paste clarity, and
lower pasting viscosity than the native starches. These results
indicate that starches treated by HMT are more thermo-
stable, and it shows lower retrogradation than the natives.
Lin et al. (2019) subjected corn, tapioca and potato
starches to HMT using cycles of heating-holding-cooling
(interaction cycle) repeated up to six times. HMT generated
differences in crystalline structure of the starches, reducing
the enthalpy and the swelling power in different order for
each starch source (potato > tapioca > corn). The authors
observed that increasing iteration and the holding time, the
same order for the treated starches was observed for the
shifting extent of pasting properties.
Bharti, Singh, and Saxena (2019) modified mango kernel
starches using HMT and evaluated its impact on morpho-
logical, structural, pasting and physicochemical properties.
HMT showed significant effect on physicochemical and
pasting properties, but slight change in surface morphology.
The authors pointed that starches treated by HMT showed
lower retrogradation rate and lower apparent amylose con-
tent than the native, and they suggest that these treated
starches are interesting to produce biodegradable films,
among other possible applications.
Finally, it is important to mention that there is another
similar process for starch modification also uses water and
heat, called annealing. The main differences between the
HMT and the annealing are the amount of water (in anneal-
ing the starches are processed in excess of water, > 40% w/
w) and the temperature (lower in annealing). However, the
annealing process is not covered in this review because this
technique is not useful in terms of energy, time, and yield,
impairing its economic interest (Alcazar-Alay and Almeida
Meireles 2015).
In this way, we can see the potential of HMT as a phys-
ical method considered effective to prepare modified
starches owing to their increased thermal stability, resistance
to shear, the paste stability, and the water and oil binding
capacities. Moreover, HMT can affect positively the ‘slowly
digestible starch’ and resistant starch content. Some reported
results are conflicting depending of starch source and HMT
conditions, such as relative crystallinity, enthalpy, swelling
power, gel firmness, amylose content solubility.
Thermal treatments in the absence of moisture:
dry heating treatment (DHT)
Dry heating treatment (DHT) is a safe and simple physical
modification method that does not result in the production
of pollutants (Oh, Bae, and Lee 2018). Chiu et al. (1998)
reported that starches when thermally treated can achieve
functionality equivalent to that obtained by chemical cross-
linking, such as treatment with phosphorous oxychloride,
but using only heat. Chemically crosslinked starches are
used in many applications where a stable-viscosity starch
paste is needed; therefore, the dry heating process would be
an alternative that has advantages in cost, time, and in the
reduction of the use of chemicals (Chiu et al. 1998). Table 2
shows some papers in literature about DHT with tempera-
tures varying between 130 until 200  C, period of treatment
varying between 1 until 20 h, and initial moisture content of
material between 7 until 13%.
Although the application of DHT has been investigated
in pure starch, there are many studies involving the

Table 2. Dry heating treatment (DHT) in different starch and flour sources.
Raw material Conditions
Waxy rice starch pure Heating (electric oven) at 130  C for
and mixed 4h
with gum Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
Proso millet flour Heating (electric oven) at 130  C for
and starch 2 h or 4 h (flour and starch)
Moisture content (MC):
Pre-treatment: MC ¼ 8%
Post-treatment: MC ¼ 5 and 3%, for
2 and 4 h of treatment, respectively
Rice starch and flour Heating (electric oven) at 130  C for
0, 2, or 4 h
Moisture content (MC):
Pre-treatment: MC ¼ 7%
Post-treatment: not determined
High amylose Heating (electric oven) at 130  C for
rice starch 0, 1, 2, and 4 h
Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
Sweet potato starch Continuous dry heat (CDH): 130  C
for 3, 6, 9, 12, 15, 18 h.
Repeated dry heat (RDH): 130  C for
3 h, then cooled at 25  C for 60 min
(1 cycle)
Evaluation: 1 – 6 cycles
Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
Waxy potato starch 110 oC for 0.5, 1.5 and 2.5 h
Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
Waxy corn starch Repeated dry heating treatment
(RDHT)
One cycle: 140  C for 4 h and then
cooled at room temperature for 1 h.
Cycles number: 1, 2, 3, 4 or 5
Continuous dry heating treatment
(CDHT): 140  C for continuous 8, 12,
16 or 20 h.
Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
Normal maize starch 130  C for 2 h
and potato starch Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: not determined
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 5
Major findings Reference
Pure rice starch: DHT promoted reduction of peak viscosity, pasting Li et al. (2013)
onset temperature, final viscosity, storage modulus, and
gelatinization temperature, but promoted an increase of degree
of crystallinity and DH.
Rice starch–xanthan mixture: modified starches showed restricted
swelling power, and greater peak viscosity, and particle size
(attributed as a crosslinking effect). Both storage and loss modulus
increased, and tan d was reduced. Gel forming ability was
strengthened.
The pasting viscosity of flour was more affected by DHT than Sun et al. (2014)
starch, and it was associated with the presence of other
compounds in the flour as protein and lipids. The treated starch
and flour showed lower pasting temperature, DH and
crystallinity, and higher peak viscosity, trough and final viscosity,
setback, and gelatinization temperature than their respective
unmodified. The effects were more pronounced as treatment
time increased.
DHT resulted in treated rice starch and flour with no significant Qiu, Cao, Xiong,
alteration in pasting temperature, however resulted in samples and Sun (2015)
with higher peak viscosity, final viscosity, trough viscosity,
crystallinity, and modification in the morphology when
compared with the untreated starch. The gels produced by
treated samples showed higher hardness, stickiness, and
cohesiveness, however lower springiness when compared with
the untreated samples. The effects were more pronounced as
treatment time increased, and the DHT was more significant for
the flour than for the starch (differentiated behavior due to the
presence of non-starchy ingredients).
DHT using 1 h of period treatment caused the most significant Oh et al. (2018)
changes in the starch sample.
Treated starch showed higher water absorption index, water
solubility, swelling power, peak viscosity, and gel strength than the
native one. For other side, DHT promoted reduction of glycemic
index, resistant starch content, and rapidly and slowly digestible
starch content.
CDH treated starch showed higher relative crystallinity, solubility, Gou et al. (2019)
swelling power, light transmittance, and thermal parameter
values than those treated by RDH, comparing the same
treatment duration. RDH treatment resulted in starches with
slightly higher rapid digestible starch content, while CDH
treatment highly influenced the structure of starch granule
surface. For both treatments (CDH and RDH), the resistant starch
content increased as cycling or treatment time increased.
DHT promoted alteration in the morphology of starch: appearance Liu et al. (2019)
of potholes and the expansion of the center of polarized cross
structure. Treated starch showed alteration of crystalline pattern
(B to B þ A type), reduction of the relative crystallinity and DH.
For other side, treated starch showed higher swelling power,
solubility, peak viscosity and pasting temperature than the
native starch. DHT promoted increase of the rapidly digestible
starch content and reduction of the resistant starch content.
Starch treated by RDHT and CDHT showed granules aggregation, Zou, Xu, Tian, and
alterations in the relative crystallinity and in the short-range Li et al. (2019)
molecular order, reduction of water absorption index, swelling
volume, viscosity and thermal parameters. For other side, this
treated starches showed higher paste clarity, the solubility, and
paste temperature of starches when compared with native
starch. RDHT showed greater impact on weakening the
resistance to shear force, decreasing transmittance of starch
paste, and increasing retrogradation degree of starch paste than
CDHT, comparing the same duration.
For both starches, DHT decreased starch molecular weight, Chi et al. (2019)
gelatinization temperature and DH. Treated potato starch: not
showed significant difference of rapidly and slowly digestible
starch, and resistant starch content when compare with the
native one. For other side, treated maize starch showed no
significant difference in relation of rapidly but higher slowly
digestible starch, and lower resistant starch content than the
maize native. Both treated starches showed reduction of DH,
gelatinization temperature, and weight-average molecular
weight when compared with the respective control starch.
(continued)
6 B. C. MANIGLIA ET AL.
Table 2. Continued.
Raw material Conditions
Cassava starch 130  C for 2 and 4 h
Moisture content (MC):
Pre-treatment: MC ¼ 13.2%
Post-treatment: MC ¼ 6.8 and 6.7%,
for 2 and 4 h of treatment,
respectively
Maize starch 140, 150, 160, 170, 180, 190, 200  C
for 2 h
Moisture content (MC):
Pre-treatment: MC <10%
Post-treatment: MC  7%
DHT: Dry heating treatment, DH: gelatinization enthalpy.
application of DHT in flours or in starch with some addi-
tives as gums (these works also are shown in this review).
Oh, Bae, and Lee (2018) investigated the effect of DHT
on the physical properties and in vitro digestibility of high
amylose rice starch. The authors observed that DHT caused
an increase of the pasting viscosity of the starch. However,
when longer heating time was applied, treated starches
showed lower pasting viscosity, hydration properties (water
absorption index and swelling power), and gel strength. In
the results of in vitro starch digestibility, DHT decreased the
rapidly digestible starch content and it also decreased the
predicted glycemic index of the high amylose rice starch.
Gou et al. (2019) compared the effect of repeated cycles
of dry heating (RDH) and continuous dry heating (CDH)
treatments on structural, physicochemical, and digestive
properties of sweet potato starch. The treatments did not
affect the original crystalline A-type pattern of sweet potato
starch. RDH treatment caused damage in the internal struc-
ture of starch granule; while the CDH may damage the
starch granules surface. The dry heating treatments resulted
in starches with lower solubility, swelling power and pasting
viscosity, however, higher light transmittance, pasting tem-
perature and gelatinization temperature than the native
starch. The results were more significant for starches treated
by CDH than those treated by RDH, but it is important to
note that RDH resulted in treated starches with higher
digestibility in vitro than those treated by CDH.
Liu et al. (2019) investigated the effects of DHT on the
physicochemical and structure of waxy potato starch. DHT
resulted in starches with changes in the morphology, in the
type of crystallite, in relative crystallinity, in the pasting
properties, in the digestibility and in the resistant
starch content.
Zou, Xu, Tian, and Li et al. (2019) investigated the
impact of repeated cycles of dry heating treatment (RDHT)
and continuous dry heating treatment (CDHT) on the struc-
tural and physicochemical properties of waxy cornstarch.
Both treatments resulted in morphology modification of the
starch granule. Samples treated by RDHT showed poorer
short-range molecular order, lower crystallinity, transmit-
tance, swelling power, and solubility than the native starch
or starch treated by CDHT.
Major findings Reference
The increase of DHT time produced a starch with higher carbonyl Maniglia, Lima,
content and bigger granule size. It also reduced the water Junior, et al. (2019)
absorption index, increased the water solubility index, affected
granule crystallinity and reduced molecular size. The longest
storage period increased gel firmness.
DHT starches resulted in gels that exhibited better printability than
the native starch, mainly for the cassava starch dry heating treated
for 4 h.
The increase of the heating temperature of the DHT resulted in Lei et al. (2020)
reduction of the molecular size, long-amylose chains, and the
crystallinity of maize starch, while the granular structure is
retained with slightly aggregation between starch particles. The
solubility of DHT starch increased, decreased the DH while
increased the heterogeneity of starch crystallites. With heating
temperature increasing, DHT reduced the overall viscosity of
starch paste.
Chi et al. (2019) studied the effects of DHT on the struc-
ture and in vitro digestibility of normal maize and potato
starches. The authors observed that DHT affected differently
each starch source in relation to the digestibility. DHT did
not affect significantly the starch digestibility nor the resist-
ant starch content of the potato starch. For maize starch,
DHT did not affect significantly the rapidly digestible starch
content; however, treated maize starch showed higher slowly
digestible starch content and lower resistant starch content
than the native one. The authors also noted that DHT
affected the thermal properties of both starches.
Maniglia et al. (2019) investigated the effect of DHT (2
and 4 h at 130  C), gelatinization conditions (temperature: 65,
75, 85, and 95  C) and hydrogel storage period (1 and 7 days
at 5  C) on printability of hydrogels based on cassava starch.
The treated starches and the hydrogels based on these starches
were evaluated in relation to their physicochemical properties,
focusing on its application for 3D printing. The authors
observed that DHT resulted in a starch with higher carbonyl
content (oxidation) and larger granule size, lower water
absorption index, higher water solubility index, lower granule
crystallinity, lower molecular size, and lower apparent peak of
viscosity. The longest storage period increased gel firmness,
and by increasing the gelatinization temperature, the gel
strength of native and starch treated for 2 h were reduced.
The authors evaluated the printability of the hydrogels based
on the native and modified starches. Starch treated by DHT
for 4 h resulted in hydrogels with the best printability. In this
way, the authors observed that using DHT, it was possible to
obtain hydrogels with enhanced pasting properties, gel texture,
and printability, thereby expanding the potential of applying
cassava starch to 3D printing.
Lei et al. (2020) investigated the effect of DHT on the
structure and physicochemical properties of maize starch.
The authors observed that DHT greatly affects the average
molecular size, chain-length distribution, and crystalline
structure of maize starch while exhibits a slight effect on
granular structure. The increase of DHT temperature
decreases the gelatinization enthalpy and produces more
heterogeneous crystallites; declines the overall viscosity dur-
ing pasting, and also reduces the “solid-like” gel property
while increases the shear resistance of gels.

Figure 1. Flow chart of the continuous PEF system (adapted from Hong et al. 2016).
Furthermore, there are several works involving DHT in
flours and starches with some additives. Some examples are
detailed below.
Li et al. (2013) evaluated the effects of DHT on the past-
ing, rheological, thermal properties, granular and molecular
structure of the pure waxy rice starch and waxy rice starch–-
xanthan gum mixtures. DHT altered the pasting and ther-
mal properties of the waxy rice starch. The gel forming
ability of the waxy rice starch was strengthened after dry
heating treatment with xanthan gum, which can be associ-
ated as a cross-linking agent.
Sun et al. (2014) evaluated the effect of DHT on the
physicochemical and structural properties of proso millet
(Panicum miliaceum L.) flour and starch. DHT had a more
significant effect on the pasting viscosity of flour than
starch, and it was attributed to the presence of the non-
starch components such as protein in the flour. DHT caused
modification in the thermal properties, crystallinity and in
the morphology of the starch and the flour.
Qiu et al. (2015) studied the effects of DHT on physico-
chemical, morphological, and structural properties of rice starch
and flour. The results revealed that the viscosity and thermal
stability of rice starch and flour increased after DHT, and the
effects were more pronounced as treatment time increased.
According to the authors, DHT had greater effects on viscosity
and structural properties of flour than those of starch; they also
associated this behavior with the presence of proteins in the
flour. The authors noted morphology modifications and the
gels based on treated starch and flour showed higher hardness,
stickiness, and cohesiveness, however lower springiness when
compared with the respective untreated flour and starch.
These results suggest that DHT could generate starches
with desirable properties as lower solubility, which is
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 7
interesting for noodle manufacture and flavor encapsulation
in sustainable release, or due to the lower retrogradation,
use in the canned and frozen food industries (Zou, Xu,
Tian, and Li et al. 2019). The DHT was also demonstrated
as an interesting alternative to improve the printability of
starches, producing stronger gels, which is interesting for 3D
food printing application (Maniglia et al. 2020). However,
DHT needs to be controlled and optimized for each starch
source, because it can damage the starch granule, resulting
in undesirable properties.
Physical modification: non-thermal treatments
Pulsed electric field (PEF)
The pulsed electric field (PEF) technique consists in the
application of short duration pulses (ls to ms) of high volt-
age to a sample located between two electrodes and submit-
ted to electric fields (general system showed in Figure 1). It
is an emerging technology to decontaminate food products
and it is also being explored to modify the structure of plant
tissues. The generation of transmembrane potential may
cause temporary or permanent permeabilization of cell
membranes through a process known as electroporation
(Zimmermann 1986). Small bacterial cells (1–10 lm) require
high electric fields for membrane permeabilization, however
plant cells need lower electric fields (1–2 kV/cm) due to
their larger size (10–100 lm) (Janositz, Noack, and Knorr
2011). The pulsed electric field (PEF) technology has been
used as a non-thermal food preservation method to inacti-
vate pathogens or spoilage microorganisms, and minimize
the loss of color, taste, nutrients, texture, and heat labile
functional components of foods (Zeng et al. 2017). Many
studies have demonstrated the advantages obtained from the
8 B. C. MANIGLIA ET AL.
use of PEF treatment, such as: nature of continuous process-
ing and uniform treatment intensity, low processing tem-
perature, short treatment time (Zhu 2018a). Moreover,
treatment via PEF has been successful to be applied for
liquid foods with low viscosity and adequate electrical con-
ductivity. In addition, it has been used to alter cell perme-
ation and to improve mass transfer processes, such as
drying (Llavata et al. 2020) and extraction (Yan, He, and
Xi 2017).
The use of PEF for starch modification is still little
explored. However, recent studies have indicated that PEF
treatments have affected differently the physicochemical
properties of starch.
The PEF system has to present an efficient temperature-
controlling unit because the high electric field leads to exces-
sive heat and unwanted electrolytic reactions. For starch
modification involving PEF treatment, the works report the
use of a water bath to control the temperature (maintaining
under 40–45  C) of the starch suspension. The samples are
placed between a set of electrodes, and the electric field can
be in the form of bipolar, square wave, exponential decay-
ing, or oscillatory pulses (Hong et al. 2016).
There is an increasing number of papers showing that
the PEF application can affect the physicochemical proper-
ties of starches – presented in Table 3.
Han et al. (2009) evaluated the PEF treatment in corn-
starch. Increasing the electric field strength, the cornstarch
was significantly deformed (rearrangement and destruction
of starch molecular structure), presented greater granules
agglomeration and reduction of the crystallinity degree, the
peak, breakdown and final viscosity. Finally, the authors
affirmed that PEF is an interesting method to modify prop-
erties of starch and get a desired product for food
application.
Han et al. (2009) evaluated the effects of PEF treatment
on physicochemical properties of potato starch. PEF resulted
in granules with higher roughness or damages, and higher
size, being more intense the effect with increasing electric
field strength. Furthermore, in the PEF treatment, with
increasing electric field strength, starch granules suffered
reduction of the relative crystallinity, the gelatinization tem-
peratures, the gelatinization enthalpy, the viscosity peak and
the breaking viscosity when compared to the native one.
The authors attributed the modification on the physico-
chemical properties of the starch due the molecular
rearrangement of granules of potato starch promoted by
PEF treatment.
Han, Zeng, et al. (2012) studied the effects of the PEF
treatment on some properties of tapioca starch. It was
observed that high energy input could destroy the crystal
region of tapioca starch. Furthermore, increasing electric
field strength promoted reduction of the gelatinization
enthalpy, the gelatinization temperature, the peak viscosity
and the breakdown viscosity. The authors concluded that
PEF can be used as a useful treatment to modify the proper-
ties of starch in order to expand its application potential in
the food industry.
Han, Yu, et al. (2012) investigated the effects of PEF
treatments on structure and thermal characteristics of maize
starch. The starch molecular weight, the gelatinization tem-
peratures and the enthalpy of gelatinization reduced with
increasing electric field strength and treatment time. It was
discussed that electric field strength played a dominant role
in PEF treatments. For other side, the authors observed that
PEF treatments not affected the chemical structure of
maize starch.
Zeng et al. (2016) investigated the effect of PEF treatment
on the granular morphology, molecular weight, semi crystal-
line structure, thermal properties, and digestibility of waxy
rice starch. These authors noted that PEF caused roughness
and pits in the starch granules and presence of aggregated,
being the effect more intense with the increasing electric
field strength. Starch treated by PEF showed lower value of
gelatinization onset temperature, peak temperature, conclu-
sion temperature, and enthalpy than native starch. The
treated starch showed lower relative crystallinity as increase
of electric field intensity. Starch treated by PEF showed
higher rapidly digestible starch level and lower slowly digest-
ible starch level when compared to the native one, therefore,
this treatment significantly affected its digestibility.
Hong et al. (2018) applied the PEF treatment in esterified
potato starch to evaluate the effects on its digestibility.
Esterified starch treated by PEF presented granules with
higher surface roughness, better glycemic digestibility and
superior emulsion stability. The results illustrate that PEF
increased the emulsification capacity and the slowly digest-
ible starch (SDS) content of potato starch granules. The
authors commented that higher SDS content would have
potential regulation for people with metabolism disorder.
Li et al. (2019) studied the PEF effect on the structural
properties and the digestibility of starches with different
crystallinity pattern type: wheat (type A), potato (type B),
and pea (type C). The authors noted that PEF treatment
could change the structure of these starch granules, being
the biggest changes in potato starch. The PEF treatment not
caused alterations in the X-ray diffractive patterns, fractal
dimension and thickness of semi-crystalline layered struc-
ture, and in the absorption peak positions on infrared spec-
tra. For other side, the authors observed that PEF treatment
could change the luminance of Maltese cross, the relative
crystallinity, the molecular weight distribution of these
starches. For the three starches treated at relatively lower
electric field intensity, in vitro digestion tests demonstrated
an increase of the portion of rapidly digestible starch, a
reduction of the slowly digestible starch content, and a
reduction of the portion of resistant starch when compared
with the natives.
Wu et al. (2019) investigated the effect of PEF treatment
in solid state on properties of japonica rice starch. The
authors noted that PEF treatment promoted modification in
the morphology of the starch granules, mainly, in outer
structure. The modified molecular structure showed one
rearrangement of short-range and slightly damage of the
amorphous and crystalline zones. This modification resulted
in a treated rice starch with higher susceptibility to the

Table 3. Pulsed electric field (PEF) treatment in different starch sources
Electric field
Raw material Conc. strength (kVcm1) Process conditions
Corn starch 8% (w/w) 30, 40, and 50 Square-wave form, unipolar;
Pulse frequency: 1008 Hz;
Pulse duration time: 40 ls;
Electrode diameter: 0.30 cm;
Electrode gap: 0.30 cm;
Sample flow rate: 60 mL.min
Suspension electric
Potato starch conductivity: 200 lScm 1 ;
Temperature below 50  C
Tapioca starch Square-wave form, bipolar;
Pulse frequency: 1kHz;
Pulse duration time: 10 ls;
Electrode diameter: 0.30 cm;
Electrode gap: 0.30 cm;
Sample flow rate: 60 mL.min
Suspension electric
conductivity: 150 lS.cm 1
Temperature below 50  C
Treatment time: 214 ls
Maize Square-wave form, bipolar;
starch Pulse frequency: 1kHz;
Pulse duration time: 10 ls;
Electrode diameter: 0.30 cm;
Electrode gap: 0.30 cm;
Sample flow rate: 60 mL.min
Suspension electric
conductivity: 150 lS.cm 1
Temperature below 50  C
Treatment time: 424, 848 and
1272 ls, separately.
Waxy rice starch 10% (w/w) 30, 40, and 50 Square-wave form, bipolar;
Pulse frequency, 1 kHz;
Pulse duration time, 40 s.
Electrode diameter: 0.30 cm;
Electrode gap: 0.30 cm;
Sample flow rate: 60 mL.min
Suspension electric
conductivity: 50 lS.cm 1
Temperature below 40-45  C.
Japonica rice starch 40% (w/w) 2.86, 5.71, Pulse frequency: 600 Hz;
and 8.57 Pulse width: 6 ls
Residence time: 90 s
Plate electrodes distance:
3.5 cm
Temperature below 50  C
Esterified – 1.25, 2.50, 3.75, Square-wave form, bipolar;
potato and 5.00 Pulse frequency, 1 kHz;
starch Pulse duration time, 40 s.
Electrode diameter: 0.30 cm;
Electrode gap: 0.30 cm;
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 9
Results Reference
Increasing electric field strength, Han, Zeng, Yu, Zhang,
the cornstarch granules showed and Chen (2009)
higher roughness or damages,
and size, reduction of the
relative crystallinity,
1
gelatinization temperatures, DH,
peak and breakdown viscosity.
As the electric field strength Han et al. (2009)
increased, the potato starch was
significantly deformed, showed
a greater agglomeration of
granules, reduced its relative
crystallinity, peak, breakage and
final viscosity.
Tapioca starch granules treated by Han, Zeng,
PEF showed dissociation, et al. (2012a)
denaturation, damage, and loss
of crystalline structure. After 50
kVcm1, crystal region of
1
tapioca starch was destroyed. As
the electric field strength
increased, treated starches
showed lower peak viscosity,
breakdown viscosity, final
viscosity, gelatinization
temperature and DH.
As the electric field strength and Han, Yu, et al. (2012)
the treatment time increased,
treated starch showed reduction
of the gelatinization
temperatures, the DH, and the
1
molecular weights. The
dominant parameter of PEF
treatment for starch
modification was the strength
of the electric field. Maize starch
treated by PEF not showed
alteration in the
chemical structure.
As the strength of the electric field Zeng et al. (2016)
increased, the treated starches
showed greater roughness and
pits in the granules, a greater
presence of aggregates, lower
1
temperature of gelatinization,
onset, peak and conclusion and
lower DH. By increasing the
intensity of the electric field, the
treated starches showed lower
relative crystallinity, a higher
level of rapidly digestible starch
and a reduction in the level of
slowly digestible starch.
PEF treatment resulted in a starch Wu et al. (2019)
with lower DH and
retrogradation of the gel. As the
electric intensity was increased,
the rapid digestible starch
increased, the slowly digestible
starch reduced and the resistant
starch content changed slightly
with the PEF treatment. Treated
starch showed damage in the
amorphous and crystalline
structure. The electric field
strength affected directly in the
DH and in the molecular weight
of amylopectin.
The starch granules treated by PEF Hong et al. (2018)
showed protrusions,
deformations, and pits on
granules surface, better stability
in the emulsion, slightly
(continued)
10 B. C. MANIGLIA ET AL.

Table 3. Continued.
Electric field
Raw material Conc. strength (kVcm1) Process conditions
Sample flow rate: 60 mL.min
Suspension electric
conductivity: 11 mS.cm 1
Temperature below 40-45  C.
Treatment time: 51 ms
Results Reference
1
reduction of crystallinity,
resistant starch content and the
rapidly digestible starch content,
but promoted increase of the
slowly digestible starch content.
The effect of PEF treatment on
the starch properties were more
pronounced as the intensity of
electric field increased.

Wheat, potato, and 40% (w/w) 2.86, 4.29, 5.71, Pulse frequency: 600 Hz; PEF treatment caused alteration in Li et al. (2019)
pea starch 7.14, and 8.57 Pulse width: 6 ls the birefringence, but not
Residence time: 90 s affected the crystalline type of
Plate electrodes distance: starch granules. Wheat and
3.5 cm potato starch treated by PEF
Temperature below 50  C showed significant alterations
on the scatter structure and
fractal dimension of self-similar
structures. Treated starch
showed alteration in the
molecular weight distribution,
and in the digestibility of
starches, especially wheat starch
and potato starch.
PEF: pulsed electric field; Conc.: concentration of the suspension; DH: gelatinization enthalpy.

digestive enzyme. Finally, the authors affirmed that PEF
treatment can be beneficial for to produce rice starch-
based food.
According to Zhu (2018a), PEF treatments to modify
starches have not been applied yet in industrial settings;
therefore it is necessary for this technology to transferring
batch process to continuous and pilot scale process.
Although PEF has been commercially used for juice produc-
tion, the volume needed for starch processing is in a differ-
ent scale. Other points such as cost estimation (such as
industrial scale installations and energy consumption) and
technical feasibility still need to be extensively evaluated.
Ultrasound (US)
The ultrasound (US) technology can be described as the
application of acoustic waves of high frequencies that are
mechanically spread in gaseous, liquid or solid systems.
Taking the human audition as reference, the “audible” fre-
quencies are classified as “sound” (20 Hz to 20 kHz).
Frequencies below that are known as “infrasound”, and
above as “ultrasound” (Carcel et al. 2012).
The US can be classified according to its intensity as “low
intensity US” (< 1 W/cm2), usually applied for nondestructive
purposes as processing control, and “high intensity US” (>
1 W/cm2), which can be used to desirably modify products
and improve processes (McClements 1995; Carcel et al. 2012).
The high intensity US is usually generated by electrical energy
provided to transducers (ceramic materials), which in turn
converts the energy into mechanical vibrations (Kentish and
Feng 2014). It is, therefore, a physical process.
The US characteristics makes it an attractive technology
for different industrial applications, and it has been consid-
ered as a “green” innovation (Chatel 2018). One of the main
reported limitation of this technology, however, is its lack of
standardization and reproducibility of scientific studies.
Important parameters and experimental conditions are not
successfully reported in the literature, and the results are
often contradictory (Chatel 2018). Even temperature control
is difficult to attain, and some works in the literature did
not deal with this with the necessary care. This can be par-
ticularly important in starch modification studies. In fact,
the results reported below regarding starch modification
using US illustrates this challenge.
The effects of the US technology on a product depend on
several factors, as the characteristics of the system, of the
product and of the US equipment. In food products, US has
being used for several purposes, as to accelerate mass trans-
fer (Fernandes, Gall~ao, and Rodrigues 2008; Miano, Ibarz,
et al. 2016; Miano, Ibarz, et al. 2016), to improve physical
properties (Rojas et al. 2016), to improve nutrients accessi-
bility (Campoli et al. 2018), to modify enzymatic activity
(Rojas et al. 2017), and to modify different polysaccharides,
including starches and starchy foods (Seshadri et al. 2003;
Iida et al. 2008; Tiwari et al. 2010; Zhu 2015).
As the starch modification processes using ultrasound are
usually performed in liquid systems (Bemiller and Huber
2015), the main US effect in this case is due to the cavita-
tion effect. When ultrasound waves pass through the prod-
uct, cycles of compression-expansion take place in the
medium (caused by the difference of pressure induced by
the acoustic waves), leading to formation and implosion of
vapor bubbles (i.e., the cavitation phenomenon) and which
dissipating a large amount of energy and shear in a local
spot, also increasing the temperature and pressure (Anese
et al. 2013). Therefore, despite being categorized as a “non-
thermal” process, the US unintentionally generates heat in a
microscale, which must be cooled if the intention of the
study is to observe only the US effects.
Moreover, the cavitation on metal surface is characterized
by high shear stress values, resulting in its erosion. It

Figure 2. General aspect of different ultrasound systems: ultrasound probe (A), sample in direct contact with the ultrasound bath (B), and sample in indirect contact
with the ultrasound bath (C) (adapted from Castanha et al. 2019).
happens in both bath reactor (in general made of stainless
still) and probe/tip reactor (in general made of titanium).
The author’s experience visiting laboratories across the
World is that equipment erosion (in special probe tip) is in
general neglected, compromising the process repeatability
and also contaminating the sample with metal particles. We
suspect these metal micro or nanoparticles can alter the
measured starch properties and/or behave as bullets during
processing, possibly damaging starch granules. These
hypotheses must be evaluated, but is worth mention the
effects must be separated.
When the acoustic cavitation occurs inside or in the
vicinity of a starch granule, it is capable of disrupt its struc-
ture. In fact, the most commonly reported results are related
to damages on the starch granules’ surfaces (as pores, cracks
and other fissures), depolymerization of molecules and some
changes in the starch properties: swelling power, solubility,
paste clarity, pasting properties and gel texture are the most
commonly reported to be affected. It is important to high-
light once again that a high variety of equipment, processing
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 11
conditions and starch sources has been evaluated in the lit-
erature, leading to some contradictory results often reported
(Bemiller and Huber 2015).
Figure 2 illustrates the general aspect of different ultra-
sound systems used for starch modification. It is important
to mention that all the equipment schematized in Figure 2
has a temperature control mechanism coupled to the system,
to illustrate their importance.
Table 4 summarizes the main findings and processing
characteristics of works using US as a physical modification
process for starches and flour.
Castanha, Lima, et al. (2019) combined ultrasound (bath
reactor) and ozone to modify corn starch (25  C). The US
treatment by itself presented little or no measurable effect
on the corn starch molecular and granular structure, nor on
the starch properties. On the other hand, when combined
with the ozone, the US improved the ozone action. The
authors discussed that this behavior can be possibly related
to internal modifications within the granules caused by the
US action, which could not be measured by the analysis
12 B. C. MANIGLIA ET AL.
Table 4. Ultrasound (US) treatment in different starch and flour sources.
Raw material Conditions
Normal, waxy and high- 100 g of starch suspension in
amylose corn starches distilled water (30%),
placed inside a beaker. US
treatment was carried out
with stirring for 30 min
at 30  C.
Potato starch Starch suspension in distilled
water (10%). The samples
were treated with different
power (60, 105, 155 W) at
a frequency of 20 kHz for
30 min. With
temperature control.
Corn starch 100 g of starch suspension in
distilled water (5%).
Samples treated for 40 min
at 30  C using different
ultrasonic frequency
(20 kHz, 25 kHz and 20 kHz
þ 25 kHz)
Rice, corn, wheat and Starch suspension in distilled
potato starches water or 99,8% ethanol
(30%, w/v). Treated with
US for 30 min at 20  C, at
a frequency of 20 kHz
Cassava starch Starch suspension in distilled
water (5%, w/v). US
treatment using 40%
amplitude during different
times (5, 10 and 20 min),
and using 60% of
amplitude for 20 min. Two
conditions were
performed: with
(immersion in an iced-
water bath) and without
temperature control.
Equipment’s information
Sonicator KQ-50DB (Kunshan,
China) with na energy
input of 100 W.
20 kHz probe (VCX 500,
Sonics, USA) using a pulse
mode set as continuous
sonification for 2 s and
pause for 2 s. Probe had a
tip of 13 mm in diameter
and was immersed in
the liquid.
Tri-frequency US device (SB-
1680DTY), supplied by
Ningbo Xinzhi Bioscience
Co., Inc (Ningbo, China),
with adjustable electric
power maximum up to
400 W for each frequency
(40 kHz, 25 kHz
and 20 kHz).
Sonoplus HD 2200
homogenizer (Bandelin
Electronic, Berlin, Germany)
at frequency of 20 kHz and
power 170 W.
Sonics VCX-750 ultrasonic
equipment (Vibra Cell,
USA), with a power of
750 W.
Major findings Reference
Pores and fissures could be observed on LLuo et al. (2008)
the surface of some treated samples
after the sonication. The crystalline
structure of the three corn starches
was unchanged after ultrasonic
treatment. On the other hand, the
sonication increased the gelatinization
transition temperatures, swelling
power and the solubility of all
samples, while decreased their DH
and their gelatinization temperature
range. The syneresis resulted from
freeze-thaw cycles increased for the
sonicated high-amylose sample, while
decreased for the other two. The
apparent viscosity patterns of the
samples remained unchanged,
however a drop on the apparent
viscosity of the high-amylose sample
was clearly observed.
Incisions and channels were observed on ZZhu et al. (2012)
the granules’ surface of the sonicated
samples, being aggravated to erosions
with increasing US power. Also, water
diffusion into starch granules was
apparently facilitated by those
erosions, implying in changes in the
cluster structure and consequently in
a molecular disorder.
The apparent viscosity of the treated HHu et al. (2015)
samples decreased after the
sonication. The sonicated granules
presented depressions on their
surfaces, especially after the treatment
using the dual-frequency US (20 kHz
þ 25 kHz).
In general, the observed results were SSujka (2017); Sujka
more expressive when the US was and Jamroz (2013)
applied in water than in ethanol. In
any case, the US treatments resulted
in cracks and depressions on the
surface of the granules of all starch
sources, as well as the natural central
cavities of the starch granules seemed
to be bigger after the treatments. The
sonication also reduced the starch-
iodine affinity and the apparent
viscosity of the samples, while
increased their solubility, swelling
power, fat and water absorption, least
gelling concentration (except for
potato starch) and their porosity (in
water). The paste clarity results were
dependent of the starch source and
solvent used.
Ultrasonic treatment without MMonroy, Rivero, and
temperature control increased the Garcıa (2018)
suspension temperature to 65  C after
20 min, causing the complete starch
gelatinization at 60% of amplitude,
and partial starch gelatinization at
40%. In general, the US caused
superficial damages on the starch
granules, increasing the surface
roughness and the formation of
cavities, channels and cracks, as well
as broadening the granular size
distribution. ATR-FTIR spectra and X-
ray diffraction results indicated that
US treatment caused a structural
disturbance in the crystalline regions
of the granules, decreasing their
(continued)

Table 4. Continued.
Raw material Conditions
Quinoa flour 10 g of quinoa flour was
suspended in 200 mL of
water. Treatment was
paused for 10 min every
1.2 h to prevent over-
heating. Treatment times:
1.2, 2.4, 4.8, 9.6, and
19.2 h. With temperature
control (below 25  C).
Corn starch US was used alone and in
combination with ozone.
The starch sample (700 mL
of starch suspension in
distilled water at 10%) was
placed inside a beaker
with mechanical stirring
and temperature control
(24-26  C). The beaker was
put inside the US bath and
treated for 8 h.
Oat starch US bath: 100 mL of starch
suspension in distilled
water (5%). Bath operating
at an intensity of 5 W/cm2
for 10 and 20 min. With
temperature control (25  C)
US probe: 100 mL of starch
suspension in distilled
water (5%). Equipment
with 20 kHz horn sonicator
at intensities of 39, 48, 63
W/cm2 for 10 and 20 min.
With temperature
control (25  C).
US: ultrasound; DH: gelatinization enthalpy; ATR-FTIR: attenuated total reflectance Fourier transform infrared.
Equipment’s information
Omni Sonic Ruptor 250 75
(Omni International,
Kennesaw, GA, USA)
equipped with an
intermediate processing tip
76 (3/8’’) (frequency of
20 kHz, power of 250 W,
and pause of 80%).
US bath model Q13/25,
Ultronique, Brazil.
Frequency of 25 kHz and
volumetric power of 72 W/
L. The bath was filled with
6 L of distilled water and
approx. 0.5 g of
dishwashing detergent, to
decrease the
surface tension.
US bath: 350 W Eurosonic 4D
US bath (Euronoda SPA,
Vicenza, Italy) having an
overall dimension of
315255165 mm (LHD)
and an output power of
350 W.
US probe: 20 kHz Topsonic
UP400-A US device (Top
Sonic Co., Tehran, Iran)
equipped with a 12 mm
Titanium horn. The probe
was placed at 1.5 cm
depth of the sample and
sonication was carried out
at different
nominal powers.
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 13
Major findings Reference
degrees of crystallinity. All those
results reflected on some properties,
by increasing the swelling power of
the samples, decreasing the DH, and
increasing the pastes’ stability under
refrigeration condition.
Treatment times higher than 5 h showed ZZhu and Li (2018)
more effect on the quinoa flour
properties. The US increased the
water solubility index, the DH and the
in vitro starch hydrolysis of quinoa
flour. On the other hand, US
decreased the swelling power, the
gelatinization temperatures, the
apparent viscosity during the paste
formation, and the hardness,
cohesiveness and springiness of the
gelled quinoa flor. Also, the US
process decreased the total phenolic
content and the in vitro antioxidant
activities of quinoa flour. The color of
the samples was also affected by the
sonication, presenting a decreased
lightness (L) and increased a
and b.
The US treatment alone had no CCastanha, Lima,
measurable effect on the corn starch et al. (2019)
molecular structure (pH, carbonyl and
carboxyl groups content, apparent
amylose content and molecular size
distribution). Also, no particular
evidence of the US action on the
starch granule’s particle size
distribution, crystallinity nor
morphology was observed, as well as
no starch property was affected by
the US. However, when the US was
combined with the ozone technology,
some properties such as the paste
clarity and pasting properties were
affected, especially when the US was
used before the ozone.
The water bath US was not able to FFalsafi et al. (2019)
cause any changes on the oat starch’s
granule surface, granule size, amylose
content, thermal properties, paste
viscosity, paste clarity, gel hardness,
starch solubility and swelling power
at the studied conditions. The
syneresis of the sonicated samples
also did not change after 5 days of
storage. On the other hand, the water
and the oil absorption increased after
20 min of sonication.
In general, especially at high intensities
(> 48 W/cm2), the US probe was able
to cause fissures and pores on the
surface of starch granules, to reduce
their sizes, to increase the amylose
content, to change the gelatinization
temperature and DH, to decrease the
degree of crystallinity, to improve the
paste clarity, to increase the water
and the oil absorption capacity and to
reduce the paste viscosity. Also, a
general increase of the samples’
solubility at high temperatures (80
and 95  C) and of their swelling
power at low temperatures (50 and
65  C) for the highest energy inputs
was observed. In general, the
syneresis increased after 3 days
of storage.
14 B. C. MANIGLIA ET AL.
performed in their work. The authors concluded, therefore,
that the US can be a useful technology to enhance the ozone
processing.
Falsafi et al. (2019) modified oat starch using both US
probe and US bath equipment, with temperature control
(25  C). The water bath presented little or no changes on
the oat starch’s structure and properties, being able to
remarkably affect only the samples’ water and oil absorption
capacity. On the other hand, the probe presented promising
results. In general, especially at the highest intensities
(>48 W/cm2), the authors observed a presence of pores and
fissures on the surface of the processed samples, while a
remarkable granular size reduction was observed. Also, in
general, the US probe treatment increased the apparent
amylose content, swelling power, solubility, water and oil
holding capacity, retrogradation tendency, syneresis and the
paste clarity of the samples, but decreased the gel hardness,
the degree of crystallinity and the enthalpy of gelatinization.
In conclusion, the authors pointed that mostly of the
observed results were modest, except the granular size
reduction at the highest intensities, mentioning that some
properties could be interesting for specific food applications.
Hu et al. (2015) studied the effect of different US fre-
quencies on the characteristics of corn starch suspension. In
general, the authors observed a decrease in the peak appar-
ent viscosity, and an improvement on their thermal stability
and retrogradation tendencies. The SEM images showed
depressions on the surface of starch granules, especially after
the treatment using the dual-frequency ultrasound (20 kHz
þ 25 kHz).
Luo et al. (2008) used US to modify different types of
corn starch (normal, waxy and high-amylose). Pores and fis-
sures were observed on the surface of some starch granules.
The treatment increased the solubility, the swelling power
and the gelatinization temperature of the samples. On the
other hand, the enthalpy of gelatinization decreased after
sonication. The syneresis observed after freeze-thaw cycles
were source-dependent, since it increased for the sonicated
high-amylose starch, while decreased for the normal and
waxy samples. The X-ray diffraction pattern was not affected
by the US, as well as the apparent viscosity patterns of the
normal and waxy corn starches. The authors concluded that
US affected mostly the amorphous regions, and the amylose
molecules were more affected than the amylopectin mole-
cules. Also, their results suggested that the US effect was
dependent of the starch amylose content.
Monroy, Rivero, and Garcıa (2018) evaluated the effect of
US treatment on cassava starch, under different US ampli-
tude, with or without temperature control. Considering the
samples processed without temperature control, it was
observed that the temperature increased to 65  C after
20 min, causing a complete starch gelatinization at 60% of
amplitude, and partial starch gelatinization at 40%.
Considering the results obtained with temperature control,
the US was proved to cause superficial damages on the
starch granules, increasing the surface roughness and the
formation of cavities, channels and cracks, as well as broad-
ening the granular size distribution. Furthermore, other
characteristics of the cassava starch were affected by US,
such as its swelling power (increased), degree of crystallinity
(decreased) and rheology (revealing a starch with higher sta-
bility under refrigeration condition, i.e., with lower tendency
to retrograde). In conclusion, the work showed the efficacy
of using the US technology to desirably modify cassava
starch, as well as illustrated the importance of controlling
the process conditions, especially the temperature.
Sujka and Jamroz (2013) used US to modify rice, corn,
wheat and potato starch suspensions, in distilled water or in
99.8% ethanol. Scanning (SEM) and transmission (TEM)
electronic microscopies showed that the US treatment
resulted in cracks and depressions on the surface of the
granules of all starch sources, especially potato and wheat.
Also, most of starch granules treated with ultrasound
showed an increase of their central cavities’ sizes. Fat and
water absorption, least gelling concentration (except for
potato starch), solubility and swelling power increased after
the treatment, while the starch-iodine affinity and the appar-
ent viscosity decreased. Regarding paste clarity, US in etha-
nol decreased paste clarity of rice and wheat starches and
did not change the paste clarity of corn and potato starches.
On the other hand, US in water had none effect on the
paste clarity of the samples, except for potato starch, which
showed an increased value after sonication. By evaluating
the same starch sources in similar conditions of US treat-
ment, Sujka (2017) observed an increase of porosity on the
specific surface area of all sonicated samples in water, and
only for the potato starch in ethanol. Considering the
results, it is possible to say that, in general, the effect of the
US in water was more expressive than in ethanol. However,
it is important to mention that the authors did not evaluate
the effect of the ethanol alone on the starch characteristics,
which is an important parameter to be considered. In con-
clusion, the US effect on the starch structure and properties
was dependent of the starch source and of the solvent used
for the modification (water or ethanol).
Zhu et al. (2012) studied the effect of different conditions
of US treatment on potato starch structural features. SEM
images showed that the treatment induced incisions and
channels on the granules’ surface, which was aggravated to
erosions as the US power increased. Those surface damages
apparently facilitated water diffusion into starch granules,
which changed the cluster structure of potato starch,
decreasing the molecular order, as proved by small-angle X-
ray scattering (SAXS). Despite that, polarized light micros-
copy and X-ray diffraction patterns showed that the effect of
the US treatment on the sample’s crystal structure was
minor, indicating that the water diffusion had a major effect
on the amylose region. The authors suggested that those
structural changes will affect functional and physiochemical
properties of the potato starch, and further studies
are necessary.
Zhu and Li (2018) evaluated the effect of US treatment
up to 19 h on quinoa flour functionality. In general, espe-
cially at treatment times higher than 5 h, the US was
reported to increase the water solubility index and the
enthalpy of gelatinization (DH), while decreased the swelling

power, the gelatinization temperatures (To, Tp, and Tc), the
apparent viscosity during the paste formation, and the hard-
ness, cohesiveness and springiness of the gelled quinoa flour.
The in vitro starch hydrolysis of quinoa flour in general
increased after US treatment. On the other hand, the US
process decreased the total phenolic content and the in vitro
antioxidant activities of quinoa flour. The starch color was
also affected by sonication, presenting a decreased lightness
(L) and increased a and b. The authors stated that the
changes were dependent of the processing time and were
related to the modification of each component of the flour
(particularly starch, according to the authors – but we sus-
pect of proteins). In conclusion, the US was proved to affect
the main functional properties of quinoa flour, such as its
cooking performance (enhanced the cooking stability and
decreased the energy necessary for cooking the flour, as
proved by the pasting results), and its water solubility, being
a good alternative for gluten free breads – according to
the authors.
To sum up, as previously discussed, the US treatment is
mainly reported to affect the starch granules’ surfaces and to
cause molecular depolymerization. Those damages can lead
to changes on the starch properties and functional charac-
teristics. However, the results regarding the starch properties
are usually contradictory, being highly dependent of the
processing conditions (equipment, solvent, temperature, etc.)
and starch source. In conclusion, all those works illustrated
Figure 3. General aspect of the ozonation system, illustrating different possibilities of reactors, being the reactors 1 and 2 designed for liquid systems, and reactor
3 for powder systems (adapted from CCastanha, Matta Junior, and Augusto, 2017).
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 15
the fact that the US technology can be used to desirably
modify starch and flour samples. However, its efficacy is dir-
ectly dependent of the equipment, the processing conditions
and the source, indicating that the results reported in the lit-
erature may not be considered conclusive.
Chemical modification: ozone
Ozone (O3) is a powerful oxidant, being considered an
environmentally friendly technology, since it quickly decom-
poses to oxygen (An and King 2009). Depending on the
application, ozone can have the GRAS (generally recognized
as safe) status for food processing (Alexandre, Brand~ao, and
Silva 2012; Gaou et al. 2005), and the oxidation using this
gas is considered a clean technology that requires limited
downstream purification processes (Chan et al. 2011). Even
so, different regulatory needs can be applied depending on
the country and application.
The interest for ozone processing of starch is increasing.
One of the first papers reporting this use was published in
1964: The paper, authored by Szymanski (1964), and it
describes the use of ozone to promote oxidation of
corn starch.
Ozone can be applied to starch in aqueous solution or in
gaseous phase. The process of oxidation, involving ozone,
can occur in different routes: direct reaction (normally in
acidic medium) between the substrate and molecular ozone,
Table 5. Ozone treatment in different starch and flour sources. 16

Ozone
generator Exposure time to
Raw material capacity Ozone application ozone (min) Gas flow (L/min) Other information Results Reference
Rice starch – Aqueous solution 15 or 30 0.17 Solutions with 20 30 min of ozone treatment resulted in rice An and King (2009)
40 g of starch w% ozone starch with the least retrogradation
(dry basis) in tendency and the highest
200 mL swelling extent.
of distilled
Corn, sago, and Ozone generation Starch 10 – Reaction vessel: Treated corn and sago starches showed Chan et al. (2011)
B. C. MANIGLIA ET AL.

Tapioca starch time (OGT): 1, Gaseous phase rotated lower average molecular weight,
3, 5, at 150 rpm however the opposite behavior for the
and 10 min tapioca starch. As ozone treatment
time increased, starches showed lower
viscosity, gels with higher Young’s
modulus, and higher retrogradation,
and DH. Corn starch was the most
susceptible to oxidation promoted by
ozone treatment.
Cocoyam and Ozone generation Starch 10 – Reaction vessel: The increase of the ozone generation time Oladebeye, Oshodi,
Yam starch time: 5, 10 Gaseous phase rotated was positive for the carbonyl and Amoo, and
and 15 min at 150 rpm carboxyl contents. Ozone treatment Karim (2013)
changed the crystallinity pattern (CA-
type for CB-type). The ozone treatment
promoted changes in swelling power,
solubility, pasting properties and
textural properties of the
native starches.
Cassava starch 13 mg/L Aqueous solution 60 – pH of solution: Ozone treatment not caused Klein et al. (2014)
200 g of starch 3.5, 6.5 and morphological differences in the
(dry basis) in 9.5 at 25  C granules surface, increased the
300 mL of carbonyl and carboxyl groups content,
distilled water and reduced the relative crystallinity of
the cassava starch. Starches treated at
pH 3.5 showed greater reduction of the
peak viscosity, breakdown, setback and
final viscosity. However, starches
treated at pH 6.5 and 9.5 favored the
cross-linking effect.
36 mg/L Aqueous solution 60 0.5 Cylindrical glass Ozone treatment promoted in the cassava Matta Junior, Castanha,
30 g of starch reactor starch formation of carbonyl and dos Anjos, Augusto,
(dry basis) in capacity: 2 L carboxyl groups, reduced the molecular and
900 mL of size of the starch polymers, increased Sarmento (2019)
distilled water the paste clarity (65%) and the
dough oven expansion capacity
(280%), and reduced the biscuit
hardness (33%).
43 mg/L Aqueous solution 15, 30 1.0 Cylindrical glass Increasing ozonation time produced a Maniglia et al. (2019)
10 g of starch reactor starch with higher carbonyl and
(dry basis) in capacity: 2 L carboxyl contents, lower pH and
100 mL of molecular size, and gels with different
distilled water behaviors (stronger and weaker than
the native ones). Starch ozonated for
30 min showed the lowest peak
apparent viscosity at all the
 temperatures and starch concentrations
evaluated, and provided the strongest
gel. At 65  C of gelatinization
temperature, hydrogels based on
native starches and starches ozonated
for 30 min showed good printability.
Hydrogels produced up to 65  C, only
starch ozonated for 30 min showed
adequate printability.
43.5 mg/L Aqueous solution Ozone (O3) 1.0 Cylindrical glass The ozone treatment resulted in starch Lima et al. (2020)
10 g of starch consumption reactor oxidized (increase of carbonyl and
(dry basis) in (amount of O3 capacity: 2 L carboxyl groups content), starch with
100 mL of that reacted reduction of the viscosity and
distilled water with the reduction of degree of retrogradation.
starch Starch treated in the conditions of
suspension): 0, 145.3 mg O3 gstarch1 resulted in
78.9, 145.3, hydrogels much stronger (280%) than
270.7 mg the native starch. Hydrogels based on
O3 gstarch1 cassava starch treated by ozone, on the
contrary to native starch, maintained
their consistency even at acidic
conditions. Treated starch showed
greater water solubility index, lower
water absorption index and higher
greater paste clarity than the
native starch.
Corn, potato, 46 mg/L Aqueous solution 15, 30 1.0 Cylindrical glass Increasing ozonation time, the samples Castanha et al. (2020)
cassava starch 10 g of starch reactor presented increase in molecular
(dry basis) in capacity: 2 L depolymerization, reduction of
100 mL of apparent viscosity during pasting,
distilled water reduction of the gel complex viscosity
(G) just after gel formation, and
reduction or increase in gel strength,
depending on starch concentration,
after cooling and storage. Granular
morphology was not affected by ozone
processing. Potato and cassava starches
treated by ozone showed similar
behaviors, however corn starch showed
opposite behavior.
Wheat starch 1,500 mg/kg Gaseous phase Flour: 45 2.5 Cylindrical acrylic Treated samples showed elevated levels Sandhu, Manthey, and
Flour: 100 g Starch: 30 container of carboxylic groups, depolymerization Simsek (2012)
Starch: 50 g (6.5 cm of starch polymers, increase of the
 29.0 cm) swelling power and breakdown, and
reduction of total carbohydrate content
in amylopectin fractions.
—— Flour 1, 10, 30 and 60 5 Ozone gas The flours treated for 30 and 60 min Li et al. (2012)
Gaseous phase capacity showed reduction of microbial
production: presence. The ozone treatment
5 g/h. increased the whiteness, the peak
viscosity, and the dough stability of
wheat starch. Noodles based on
treated flour showed higher firmness,
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION

springiness, and chewiness, lower

adhesiveness, delayed in the microbial
growth and in the darkening rate.
(continued)
17
Table 5. Continued. 18
Ozone
generator Exposure time to
Raw material capacity Ozone application ozone (min) Gas flow (L/min) Other information Results Reference
4.2 mg/kg Aqueous solution 15, 30, and 60 0.103 500 mL glass Ozonated starch samples showed lower Çatal and Ibanoǧ
10 g of starch bottles at 5  C pasting temperature, lower lu (2014)
(dry basis) in retrogradation tendency, and lower
100 mL of breakdown viscosity, as compared to
distilled water that of native starch. The treated
wheat starch showed higher shear-
B. C. MANIGLIA ET AL.

thinning behavior and gelatinization

grade than the control starch.
60, 120 and Aqueous solution 60, 120, and 180 33.34 Temperature The wheat starches not showed significant Goze, Rhazi, Pauss,
180 mg/L 2, 4, 6 mL of (22  C) and modifications in experimental and
grain in 100 mL pressure conditions used in the ozone Aussenac (2016)
of distilled water (0.4 bar) treatment, only a slight oxidation
reactor noticed by the increase of carboxyl
groups content.
—— Whole grain 5, 15, 25, 35, 5 Ozone As ozonation time increased, the treated Obadi et al. (2018)
Gaseous phase and 45 gas capacity starch showed higher water and oil
300 g in flask production: absorption, solubility, and swelling
of 2000 mL 5 g/h power, however reduction in the peak,
trough, breakdown, final, and setback
viscosity values. The structures of
starch and proteins were affected by
the ozone treatment.
Potato starch 47 mg/L Aqueous solution 15, 30, 45, and 60 0.5 Cylindrical glass As ozonation time increased, the treated Castanha, da Matta
10 g of starch reactor starch showed higher carbonyl, Junior, and
(dry basis) in capacity: 2 L carboxyl and reduction of sugar Augusto (2017)
100 mL of contents, pH, apparent amylose
distilled water content and molecular size. The
samples treated by ozone showed
alterations in the granule morphology,
paste clarity, and gel texture, but no
significant changes in the relative
crystallinity.
Modified starch showed reduction in the Castanha, Santos,
diameter of the larger starch granules Cunha and
and higher rapidly digestible starch Augusto (2018)
content. Ozone treatment for 15 and
30 min promoted increase of the
apparent viscosity, increase of the gel
strength (gelatinization at 65 and
70  C), and increase of the capacity of
water retention at mild temperatures
(60  C) of the potato starch.
Maize starch 42 mg/L Aqueous solution 15 1.0 Cylindrical glass Ozone treatment resulted in maize starch Castanha, Lima,
10 g of starch reactor with higher carbonyl and carboxyl et al. (2019)
(dry basis) in capacity: 2 L content, lower pH and molecular size,
100 mL of higher solubility, paste clarity, and
distilled water pasting viscosities, lower relative
setbacks. The gels produced using the
treated starch resulted in harder and
less elastic gels. It was observed
changes on the crystalline domain, on
the granules’ morphology, sizes and
shapes of the treated starches.
DH: gelatinization enthalpy.

or by indirect reaction (normally in alkaline medium) (Kim,
Yousef, and Dave 1999). The general aspect of the ozonation
system is shown in Figure 3.
Table 5 shows some works in the literature with ozone
treatment in flour and starch, with the aim of improving
their functionality.
An and King (2009) evaluated the effects of ozonation
and the addition of amino acids on pasting properties of
rice starches. The rice starch treated by ozone showed
higher swelling power of granule, and lower retrogradation
tendency and pasting property during cooling, lower cook-
ing stability, more viscous hot paste, and less rigid cooled
paste than the native starches. The authors noted that the
pasting properties of the ozonated rice starch exhibited simi-
lar behavior of oxidized starch using the chemical oxidizing
reagent sodium hypochlorite (0.8%). Finally, in this work
was reported that ozone treatment for starch modification
may result in new ingredients, expanding the various func-
tionalities of this source without using typical chemical
reagents to promote the starch modification.
Chan et al. (2011) characterized the effects of ozone treat-
ment on the molecular, rheological, mechanical, and thermal
properties of corn, sago, and tapioca starches at different
ozone generation times (OGTs). They noted the ozone treat-
ment was able to oxidize the starches, but the extension of
the oxidation was different for each source. In this way, the
ozone treatment in the same conditions resulted in different
effects on the molecular structure and rheological properties
for each starch evaluated. The differences can be associated
with the oxidation grade (formation of carbonyl and carb-
oxyl groups), but also due different rates of degradation of
amorphous and crystalline lamellae promoted by ozone
treatment for each starch.
Oladebeye et al. (2013) investigated the functional, ther-
mal and molecular behavior of native starches from coco-
yam (Colocasia esculenta) and yam (Dioscorea spp.) cultivars
modified via ozone-oxidation. This study shows that ozone
treatment affects the functional, thermal and molecular
properties of the various starches when treated under the
same conditions. The authors observed that when the ozone
treatment was applied for 10 min, the treated starches
showed properties similar of starches oxidized using conven-
tional alkaline methods. It was mentioned the importance of
this alternative oxidant method to obtain modified starch,
because it can expand the starch functionalities which is
interesting for the ever-increasing demand for starch in food
and non-food applications.
Klein et al. (2014) evaluated the ozone oxidation of cas-
sava starch in aqueous solution at different pHs. The
authors did not observe effect of the ozone treatment on the
morphology of the granules surface. It was noted that the
pasting properties were affected by the ozone treatment dif-
ferently in each pH evaluated. The starch suspension at pH
6.5 and 9.5, during the ozone treatment, favored the cross-
linking between depolymerized starch molecules. For other
side, starch suspension at pH 3.5 resulted in treated cassava
starch with the lowest peak viscosity, breakdown, setback
and final viscosity.
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 19
Matta Junior et al. (2019) treated the cassava starch with
ozone to improve the oven-expansion property. The authors
noted that the ozone treatment resulted in starches oxidized
(formation of carbonyl and carboxyl groups) and with lower
molecular size. It was also observed better oven expansion,
increase of paste clarity, and softer texture. The authors
affirmed that ozone processing is a useful alternative to the
conventional process (fermentative) used to obtain starch
with higher oven-expansion capacity.
Maniglia et al. (2019) explored the modification of cas-
sava starch by using ozone technology and evaluating the
potential of the hydrogels obtained for 3D food printing.
The authors demonstrated that ozone treatment is a relevant
strategy for modifying cassava starch intended for 3D print-
ing. Ozone processing promoted starch oxidation, reduced
starch molecular size (depolymerization), and the starch
ozonated for 30 min exhibited the lowest peak apparent vis-
cosity. The gels produced by native and starches ozonated
for 30 min presented good printability when the gelatiniza-
tion temperature used was 65  C. Up to this temperature,
starch ozonated for 30 min produced more printable gels.
The gels produced by starch ozonated for 15 min did not
present good printability. Finally, ozone processing can be
an alternative for obtaining starches with new and poten-
tially interesting properties, thereby expanding the potential
of using cassava starch in 3D printing.
Lima et al. (2020) evaluated the effect of ozone process
condition (amount of ozone that reacted with the starch sus-
pension) on the structure and properties of cassava starch.
Increasing ozone consumption, cassava starch showed higher
oxidation levels (increase of carboxyl and carbonyl content)
and reduction of large and branched molecules with conse-
quent increase of smaller sized molecules. The ozone treat-
ment with the highest amount of ozone (O3) that reacted
with the starch suspension (270.7 mg O3 gstarch1) showed
the lowest peak apparent viscosity, however for the condi-
tion 145.3 mg O3 gstarch1 resulted in cassava starch gels
much stronger (280%) than the native cassava starch. The
authors also evaluated the gel firmness for the starches in
acid conditions. They observed that hydrogels based on cas-
sava starch treated by ozone, on the contrary to native
starch, maintained their consistency even at acidic condi-
tions. Moreover, it was observed that the treated starch
showed greater water solubility index, lower water absorp-
tion index and greater paste clarity than the native starch.
In this way, the authors concluded that the structural
changes significantly influenced the starch properties and it
brings new possibilities for cassava starch application.
Castanha et al. (2020) compared corn, cassava, and
potato starches treated by ozone processing under the same
conditions. The authors observed that all treated starches
showed molecular depolymerization but each starch source
showed difference in relation to their molar mass dispersity.
Ozone process not affected the granular morphology, but
reduced the apparent viscosity during pasting and reduced
the complex modulus (G) of the hydrogels based on these
treated starches. Hydrogels based on treated starches showed
reduction or increase in gel strength, depending on starch
20 B. C. MANIGLIA ET AL.
concentration, after cooling and storage. Cassava and potato
starches showed similar behavior when treated by ozone,
however corn starch showed an opposite behavior. Finally,
these authors concluded that ozone processing conditions,
starch source and analysis conditions showed influence on
the samples’ behavior and in the functional properties.
In 2012, Sandhu, Manthey, and Simsek published an art-
icle about how the ozone gas affects physical and chemical
properties of wheat starch isolated or in the wheat flour.
Both treated starches evaluated (isolated and in the flour)
showed similar chemical and physical properties. The treated
starches showed elevated levels of carboxylic groups, higher
swelling power and the breakdown viscosity, and lower total
carbohydrate content in amylopectin fractions than the
native starch. In addition, the ozone treatment did not affect
the granule morphology and crystallinity of the wheat starch
(isolated or in the flour).
Li et al. (2012) evaluated the effect of the ozone treatment
in the quality characteristics of wheat flour and shelf-life of
fresh noodles. Results showed that treated wheat flour
showed reduction of microorganisms, and improved flour
and noodle sheet whiteness, dough stability and starch vis-
cosity properties. Moreover, the treated flour showed high
molecular mass protein aggregates. The authors also men-
tioned that from treated wheat flour was possible to produce
fresh noodles with shelf-life largely extended, evaluated by
the microbial growth and darkening rate.
Çatal and Ibanoǧ lu (2014) studied the effect of ozone
treatment on the pasting, rheology, and gelatinization prop-
erties of wheat starch. The authors noted that the treated
wheat starch showed lower breakdown (higher cooking sta-
bility) and setback viscosities (lower retrogradation ten-
dency), and higher shear-thinning behavior than the native
starch. Another point is that the ozone treatment resulted in
a wheat starch with higher degree of gelatinization (deter-
mined using enzymatic method) than the native starch.
Goze et al. (2016) evaluated the starch properties after
ozone treatment applied in wheat grains. The authors made
ozone treatment using different conditions involving the
parameters: ozone inlet concentration, humidification rate,
and reaction time. The starch isolated from the treated
grains not showed significant difference in the physicochem-
ical, rheological, and thermal properties, molecular weight
distribution and amylopectin branched chain length distri-
bution. However, the ozone treatment promoted a slight
oxidation in the wheat starch identified by the appearance
of carboxyl groups which showed increase as the ozone
treatment increased.
Piechowiak, J ozefczyk, and Balawejder (2018) explored
the impact of ozone treatment of wheat flour on the activity
of selected enzymes. The authors evaluated different ozone
concentration in the fluidized bed reactor and time of pro-
cess. As increased the ozone concentration and the process
duration, the treated flours showed lower total activity of
amylases, proteases and lipases. In this way, these authors
reported the ozone treatment as one interesting process to
control the enzymatic activity of flours.
Obadi et al. (2018) examined the effects of ozone treat-
ment on the physicochemical and functional properties of
whole grain flour. These authors concluded that the ozone
treatment resulted in modification of physicochemical and
functional properties, increasing swelling power, the water
and oil absorption capacities, and solubility, and decreas-
ing the pasting properties with increasing ozonation time.
Microscopic analysis indicated that treated flour showed
changing in the starch and proteins structures. The
authors concluded that ozone treatment is a useful and
quick tool to modify flour properties, being an interesting
alternative to chemical oxidation, such as chlorination,
which is time-consuming.
Castanha, Matta Junior, and Augusto (2017) studied the
modification in the functional and structural properties of
the potato starch using the ozone technology. The ozone
treatment in aqueous solution successfully oxidized the
potato starch, and the authors proposed, in this work, a
mechanism of action of the ozone in the starch molecules.
The treated starch showed significant changing in the past-
ing properties, gel texture and paste clarity, proving the
effectiveness of using ozone as an efficient oxidizing agent
for starch modification.
Castanha et al. (2018) evaluated the effect of ozone
treatment on properties of potato starch and discussed dif-
ferent possibilities of industrial application. The authors
observed that treated potato starch showed higher apparent
viscosity, gel strength, and higher enzymatic susceptibility
if compared to the native sample. On the other hand, the
starch ozonized for longer period were able to gelatinize at
small temperatures and were more soluble if compared to
the native and the samples ozonized for a shorter period.
They suggested that the modified potato starches can be
used in process/products that demand specifically condi-
tions such as viscous pastes or higher water retention at
moderate temperatures.
Castanha, Lima, et al. (2019) evaluated the combination
of ozone and ultrasound technologies to modify maize
starch. In this study, they evaluated also the ozone treatment
alone in the maize starch. These authors observed that the
modified starch exhibited significant changes on the starch’s
molecular structure (pH, carbonyl and carboxyl groups,
apparent amylose content, and molecular size distribution)
and properties (water absorption and water solubility
indexes, pasting properties, gel strength and paste clarity).
On the other hand, some maize starch properties were not
affected by the ozone treatment (particle size distribution,
the surface morphology, and crystallinity).
By this way, the ozone treatment can be successfully used
for the modification of starches, expanding its application
potential. However, it is important to emphasize that the
botanical source (the structure of starch) and the reaction
parameters have a great influence on the ozone action, and
further studies in this field are still required. Another fact is
that the industrial facility of ozone technology remains to be
developed for large-scale treatment of related products,
requiring inputs from different disciplines.

Table 6. Advantages and disadvantages of starch treatments
Method Advantages
HMT
Simple process
DHT
Simple process

Drying process is not necessary
PEF
Short time

Less energy consumption

Low temperature

No production of residues
US
Simple process

No chemicals are needed

No residues are produced
Ozone
Short time

Low temperature
HMT: heat moisture treatment; DHT: dry heating treatment; PEF: pulsed electric field; Ultrasound
Final remarks and perspectives
Beyond the information obtained from the performance of
methods for modifying the properties of starches, each treat-
ment shows some advantages and disadvantages that has
also to be considered to define the most suitable for the
modification of starch. Table 6 shows briefly some advan-
tages and disadvantages of starch modification techniques
discussed in this review.
The treatments mentioned and the results observed in
the literature were elaborated in small-scale, based on
laboratory tests. Therefore, in spite of the advantages of
these starch modification treatments in relation to the con-
ventional, it is still necessary investigate an increase in scale
or even the possibility of a continuous process using these
techniques. In future perspectives, information about the
cost estimation (e.g. energy consumption and building up
the facility on industrial scale) and technical feasibility are
also needed.
Finally, it is notable that the starch industry is in constant
expansion, and modification processes increase its versatility.
Allied to this, there is a growing search for more sustainable
methods that do not harm the environment. Therefore, the
“green” methods here described will certainly be interesting
alternatives to enhance starch industry.
Conclusion
There is a current trend by improvement of techniques and
processes using innovative “green” methods for starch modi-
fication. Beside promoting changes in the physical, morpho-
logical, and rheological properties, bringing new
functionalities that are not found in native starches, these
methods have the advantage of not using chemical reagents.
In this way, these methods eliminating the need for effluent
treatment and therefore there are considered as environmen-
tally friendly. The production of modified starches is an
alternative that has been developed in order to overcome
limitations of the native starches and thus increase the use-
fulness of this carbohydrate in industrial applications. Major
changes include freeze–thaw stability, paste viscosity, gelatin-
ization temperature, shear stability, swelling power,
CRITICAL REVIEWS IN FOOD SCIENCE AND NUTRITION 21
Disadvantages

High energy consumption

High temperature

Drying process is necessary

Long time

High energy consumption

High temperature

Long time

Drying process is necessary (liquid-phase)

Temperature control is required

Little-known process

Increase the sample’s temperature

Lack of standardization and reproducibility

Highly dependent of the characteristics of the system and of the equipment

Drying process can be necessary (although it can be conducted right after wet milling)

Ozone cannot be stored and must be produced in the moment to be used
solubility, changes in polymorphism, and gel firmness.
Finally, although of the good performance of these treat-
ments, it is still necessary to know better the possibility to
use it in large-scale, and thus apply in starch modifica-
tion industries.
Disclosure statement
The authors declare that they do not have any conflict of interest.
Funding
The authors are grateful to the Region Pays de la Loire/RFI “FOOD 4
TOMORROW” for funding the Post-doctoral fellowship “STARCH-
3D” of B. Maniglia; to the S~ao Paulo Research Foundation (FAPESP,
Brazil) for funding the project n 2019/05043-6; to the National
Council for Scientific and Technological Development (CNPq, Brazil)
for funding the productivity grant of P.E.D. Augusto (306557/2017-7);
this study was financed in part by the “Coordenaç~ao de
Aperfeiçoamento de Pessoal de Nıvel Superior - Brasil (CAPES)” -
Finance Code 001, through the N. Castanha Ph.D. scholarship.
ORCID
Bianca C. Maniglia http://orcid.org/0000-0003-4174-5474
Nanci Castanha http://orcid.org/0000-0002-0620-8545
Patricia Le-Bail http://orcid.org/0000-0002-3764-9765
Alain Le-Bail http://orcid.org/0000-0001-6132-5392
Pedro E. D. Augusto http://orcid.org/0000-0001-7435-343X
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