Effects of ultrasonic and chemical dual modification treatments on the structural, and properties of cornstarch

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Food Chemistry 451 (2024) 139221

Available online 2 April 2024

Effects of ultrasonic and chemical dual modication treatments on the

structural, and properties of cornstarch

Mingyu He , Xixi Wu , Tian Gao , Le Chen , Fei Teng

, Yang Li

College of Food Science, Northeast Agricultural University, Harbin, Heilongjiang 150030, China

ARTICLE INFO

Keywords:

Cornstarch

Ultrasonic

Oxidation

Esterication

Cross-linking

ABSTRACT

This study aimed to explore the changes in the structural and functional properties of cornstarch modied by

oxidation, esterication, and cross-linking under ultrasonic pretreatment. FT-IR and XRD characteristic peaks

revealed successful access to chemical functional groups. Both ultrasonic and the three chemical treatments

eroded the surface of starch granules, reducing their particle size and increasing their RC. Meanwhile, the

destruction of the granules was further enhanced by the dual modication treatments. The ultrasonic pretreat-

ment synergized and improved the swelling power, solubility, and translucency of all three chemical treatments.

Further, it improved the poorer freeze-thaw stability of cross-linked starch, resulting in a lower water precipi-

tation rate. In addition, both ultrasonic and chemical treatments signicantly decreased RDS and SDS, and

increased RS content. The ultrasonic–chemical dual modication had a synergistic effect on in vitro digestibility,

resulting in a further increase in RS. In conclusion, this study provided ideas for developing new starch modi-

cation technology and deep processing of cornstarch, expanding its application areas and thus meeting the

different needs of starch-based products.

1. Introduction

Starch, the primary source of carbohydrate intake for humans, is a

versatile, cost-effective, easily available, biodegradable, and renewable

polysaccharide polymer that has received signicant attention from

researchers (Kong, Niu, Sun, Han, & Liu, 2016). Cornstarch, a major

variety of starch, accounts for 80% of the world's total starch (Liu et al.,

2014). It serves not only as a direct consumable but also as a vital in-

dustrial raw material widely used in various sectors such as food, sugar

production, fermentation, medicine, papermaking, chemical industry,

and so forth. Cornstarch contains approximately 72% amylopectin and

28% amylose, and is a white, odorless powder. In addition, cornstarch

has the characteristics of high gelatinization temperature, high moisture

absorption, and low blood glucose index (Wang et al., 2023). However,

natural cornstarch is limited applicability in food and industry due to its

low solubility in cold water, poor thermal stability, weak shear resis-

tance, and weak gel strength (Kong et al., 2016). Therefore, starch is

modied through physical, chemical, enzymatic, and genetic modi-

cations to expand its applications so as to overcome these drawbacks and

improve the functional qualities of starch (Radi, Abedi, Naja, & Amiri,

2022).

Chemical modication techniques (such as oxidation, esterication,

grafting, and cross-linking), introduce functional units into the starch

molecule and alter the free hydroxyl groups at the C

, C

, and C

posi-

tions on the anhydrous gluconoacyl units (Aaliya et al., 2022; Sun et al.,

2017). The oxidation treatment of starch is mainly carried out at specic

temperatures and pH levels (Aaliya et al., 2022). Among these, H

breaks down quickly into oxygen and water without creating any haz-

ardous byproducts (Isbell & Frush, 1987). H

oxidation resulted in

depolymerization of starch polysaccharide chains, decreased crystal-

linity, reduced viscosity, and increased stability of the starch paste

(Aaliya et al., 2022). However, when H

oxidation was used to pre-

pare oxidized starch with high carbonyl content, an increase in the

amount of oxidant added led to a greater degree of starch degradation

and a lower yield (Zhang, Wang, Zhao, & Wang, 2012). Octenyl succinic

anhydride (OSA) acylated the modication of natural starch under

alkaline conditions, where hydrophobic OSA groups were introduced

into hydrophilic starch molecules to obtain modied starch with

amphiphilic properties (Kurdziel, Kr´

olikowska, Łabanowska, Pietrzyk,

& Michalec, 2020). OSA-modied starch can increase starch viscosity

and improve its freeze-thaw stability and digesting characteristics (Sri-

prablom, Tatikunakorn, Lerdpriyanun, Suphantharika, &

* Corresponding authors at: College of Food Science, Northeast Agricultural University, Harbin 150030, China.

E-mail addresses: tengfei@neau.edu.cn (F. Teng), yangli@neau.edu.cn (Y. Li).

Contents lists available at ScienceDirect

Food Chemistry

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

https://doi.org/10.1016/j.foodchem.2024.139221

Received 6 December 2023; Received in revised form 10 March 2024; Accepted 31 March 2024

Food Chemistry 451 (2024) 139221

Wongsagonsup, 2023). OSA has been approved by the FDA for use as a

starch modier in food products at a maximum allowable level of 3.0%

(w/w, amylose-based) (Sriprablom et al., 2023). Therefore, strategies to

enhance the starch esterication reaction of OSA are urgently needed to

further improve the starch properties. Cross-linking, the most commonly

used method for chemically modifying starch, involves creating inter-

and intramolecular linkages by guiding functional groups through

different cross-linking agents to random positions on the hydroxyl

groups of the starch molecule (Radi et al., 2022). As nontoxic cross-

linkers for starch, sodium tripolyphosphate (STPP) and sodium trime-

taphosphate (STMP) offer advantages such as safe manufacturing, gentle

synthesis conditions, high reaction efciency, and cost-effectiveness

(Gao, Li, Bi, Mao, & Adhikari, 2014). Meanwhile, phosphorylation

cross-linking–modied starch reduces heat, acid, and shear sensitivity,

increases structural and thermal stability, and exhibits good gel char-

acteristics (Sriprablom et al., 2023). However, previous studies have

shown that cross-linked starch faces challenges related to poor freeze-

thaw stability and regrowth resistance (Sriprablom et al., 2023).

Ultrasonication is extensively used for starch modication as a green,

safe, and efcient physical treatment technology (Wang et al., 2022).

Ultrasonic action on aqueous starch solutions leads to cavitation, a

process where bubbles are generated in the suspension medium and

undergo periodic compression and expansion due to ultrasonic oscilla-

tory action. These bubbles bombard the starch granules, causing shear

forces upon collapse. The rapidly rupturing bubbles lead to the

destruction of starch granules and the exposure of more reaction sites.

The reaction is accelerated and accompanied by free radical effects,

energetic mechanical effects, and thermal effects (Chavez-Esquivel,

Cervantes-Cuevas, & Vera-Ramírez, 2022). However, studies on the

compound modication of cornstarch using chemical modifcornication

and ultrasound are limited. In addition, the dual modication of starch

has become increasingly popular in response to the inability of a single

modication to fully satisfy the specic needs of starch properties for

food and industrial applications.

This study compared the effects of ultrasonic treatments and three

chemical modications on the microstructure, molecular structure, and

functional properties of cornstarch. We aimed to develop methods to

improve the functional properties of starch and provide a reference for

broadening the applications of cornstarch by exploring the relationship

between the changes in the physicochemical properties of starch

induced by the dual modications and the structure.

2. Materials and methods

2.1. Materials

Cornstarch (23% amylose and 77% amylopectin) was obtained from

Yuanye Biotechnology Co., Ltd. (Shanghai, China). All other chemicals

were analytical grade.

2.2. Preparation of modied cornstarch

The cornstarch powder was dissolved in deionized water, stirred

magnetically at 500 rpm for 2 h at room temperature, and left to stand

for 12 h at 4 ◦C to prepare a certain concentration of cornstarch stock

solution for use.

2.2.1. Ultrasonication of cornstarch

The cornstarch stock (4% (w/v)) was sonicated in a probe-type

sonicator (JY98-IIIDN; Xiangfan Instrument Co., Ltd., Shanghai,

China). After ultrasonication, the starch suspension was centrifuged at

6000 rpm for 15 min. The starch precipitate was dried in a hot air oven

at 50 ◦C (Khurshida, Das, Deka, & Sit, 2021).

2.2.2. Oxidation of cornstarch

Cornstarch was oxidized with H

by following the method

proposed by Sangseethong, Termvejsayanon, and Sriroth (2010). The

cornstarch stock solution was prepared at a concentration of 35% (w/v),

and its pH was adjusted to 8.5 using 1 M NaOH. Further, 0.05% ferrous

sulfate (on a dry starch basis) was added to the starch solution as a

catalyst. The starch solution was stirred in a water bath at 45 ◦C and the

solution was added dropwise for 10 min to reach a nal concen-

tration of 5%. It was kept at pH 8.5 for 3 h. After that, 1 M HCl was added

to stop the reaction and bring the pH down to 6.5. The starch suspension

was washed thrice with distilled water and nally with anhydrous

ethanol. The oxidized starch was dried overnight at 50 ◦C in a vacuum

oven, followed by grinding, sieving, and storing in an air-tight container.

2.2.3. Esterication of cornstarch

Cornstarch was modied by esterication with OSA following the

method of Hui, Qi-he, Ming-liang, Qiong, and Guo-qing (2009) with

minor modications. The cornstarch stock solution was prepared at a

concentration of 35% (w/v), and its pH was adjusted to 8.5. Also, 3%

OSA (on a dry starch basis) was added for 1 h and treated at 35 ◦C for 2 h.

After that, 1 M HCl was added to stop the reaction and bring the pH

down to 6.5, followed by washing and drying in the same way as in the

case of oxidized starch.

2.2.4. Cross-linking of cornstarch

Cornstarch was cross-linked with STPP and STMP following the

method of Park et al. (2018). Cornstarch stock solution (35% (w/v)) was

added to 10% sodium sulfate (on a dry starch basis) and 10% STPP/

STMP (99:1) mixture (on a dry cornstarch basis). The pH of the mixed

solution was adjusted to 11.0, and placed in an oscillating water bath at

45 ◦C for 3 h. The pH was adjusted to 6.5 with 0.1 M HCl, followed by

washing and drying in the same manner as in the case of oxidized starch.

2.2.5. Dual-modication of cornstarch

Dual-modied starches were prepared by ultrasonic pre-treatment

followed by oxidation, esterication, and cross-linking of ultrasoni-

cally modied starches (as described in Sections 2.2.2, 2.2.3, and 2.2.4).

The names of the samples are listed in Table 1.

2.3. Determination of the degree of modication

The degree of oxidation was determined by measuring the total

starch carbonyl and carboxyl group contents using the method proposed

by Zhang et al. (2012). The degree of substitution was the average

number of substituted hydroxyl groups per glucose unit and was

Table 1

Names of starch treated by ultrasonic alone and by ultrasonic-chemical dual

treatment.

Samples Ultrasonic power (W) Ultrasonic Time (min) Chemical treatment

0-CS – – –

U1-CS 200 10 –

U2-CS 200 20 –

U3-CS 400 10 –

U4-CS 400 20 –

O-CS – – oxidation

U1-O-CS 200 10 oxidation

U2-O-CS 200 20 oxidation

U3-O-CS 400 10 oxidation

U4-O-CS 400 20 oxidation

E-CS – – esterication

U1-E-CS 200 10 esterication

U2-E-CS 200 20 esterication

U3-E-CS 400 10 esterication

U4-E-CS 400 20 esterication

C-CS – – crosslinking

U1-C-CS 200 10 crosslinking

U2-C-CS 200 20 crosslinking

U3-C-CS 400 10 crosslinking

U4-C-CS 400 20 crosslinking

M. He et al.

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