Comparison of structural and in vitro digestive properties of autoclave-microwave treated maize starch under different retrogradation temperature conditions

3.0 科研～小助 2025-09-01 4 4 3.59MB 8 页 1知币

International Journal of Biological Macromolecules xxx (xxxx) xxx

Please cite this article as: Jiani Jiang et al., International Journal of Biological Macromolecules, https://doi.org/10.1016/j.ijbiomac.2024.132410

Comparison of structural and in vitro digestive properties of

autoclave-microwave treated maize starch under different retrogradation

temperature conditions

Jiani Jiang

, Wenfang Han

, Siming Zhao

, Qiongxiang Liu

, Qinlu Lin

, Huaxi Xiao

Xiangjin Fu

, Jiangtao Li

, Kangzi Ren

, Huanghua Lu

National Engineering Research Center of Rice and Byproduct Deep Processing, College of Food Science and Engineering, Central South University of Forestry and

Technology, Changsha 410004, China

College of Food Science and Technology Huazhong Agricultural University, Wuhan 430070, China

Hunan Province Grain and Material Research Design Institute, Changsha 410201, China

ARTICLE INFO

Keywords:

Temperature-cycled retrogradation

Autoclaving-microwave treatment

In vitro starch digestibility

ABSTRACT

Retrogradation is a critical step in the physical production of resistant starch. This study aimed to examine the

effects of isothermal and temperature-cycled retrogradation on the structural, physicochemical properties, and

digestibility of resistant starch type-III (RS3) under various thermal conditions. To create RS3, normal maize

starch (NM) and Hylon VII (HAM) were treated by autoclave-microwave and then retrograded at isothermal

(4 ◦C) or various temperature conditions (4/10 ◦C, 4/20 ◦C, 4/30 ◦C, 4/40 ◦C, and 4/50 ◦C). We found that

temperature-cycled retrogradation possessed greater potential than isothermal retrogradation for producing

short-range ordering and crystalline structures of RS3. Also, retrograded starch prepared via temperature cycling

exhibited higher double helix content, lower amorphous content, reduced swelling power, and less amylose

leaching in water. Furthermore, the starch digestibility was affected by structural alterations, which were more

signicant in HAM-retrograded starch. While, HAM-4-40 (39.27 %) displayed the highest level of resistant starch

(RS).

1. Introduction

Starch is the most important carbohydrate in the human diet and

extensively utilized in the food industry [1,2]. Resistant starch, an un-

digested fraction of starch in the small intestine, plays a signicant role

in preventing diabetes, enhancing gut health, and reducing the risk of

cardiovascular diseases [3–5]. Based on differences of the preparation

methods, the RS can be categorized into ve different types: RS1 -

physically inaccessible starch; RS2 - granular starch; RS3 - retrograded

starch; RS4 - chemically modied starch; and RS5 - starch-lipid com-

plexes [6]. Among them, RS3 displays excellent physicochemical prop-

erties (superior enzyme resistance, safety, and stability) [7]. Notably, as

an important step in the preparation of RS3, retrogradation is an inev-

itable phenomenon when cooked starch or starchy foods are cooled and

stored [8]. Its essence is the reorganization of disordered starch mole-

cules after gelatinization to form an ordered microcrystalline structure

[9,10]. According to the classical kinetics model of polymer

crystallization, starch retrogradation involves three sequential phases:

(i) nucleation; (ii) propagation or growth of crystals; and (iii) maturation

or crystal perfection [11,12]. The rate of crystallization throughout the

process has been primarily determined by the rst and second steps.

Several previous studies have demonstrated that these processes are

affected by various internal factors, such as amylose and amylopectin,

along with other dietary components, and external factors including

temperature, retrogradation time, and moisture content [7,13].

Temperature plays a crucial role in the starch retrogradation [10].

Typically, nucleation is favored around the glass transition temperature

of starch molecules, while crystal growth is enhanced near the melting

temperatures of the crystallites [9,14]. The cycling between these two

temperatures during the storage of gelatinized starch may accelerate

retrogradation. It has been reported that cycling between the appro-

priate nucleation and propagation temperatures over a specic period

can foster the growth of crystalline regions and the perfection of crys-

tallites [9,15,16]. Consequently, we hypothesized that temperature

* Corresponding authors.

E-mail addresses: hwfay@vip.163.com (W. Han), ljthyd@163.com (J. Li).

Contents lists available at ScienceDirect

International Journal of Biological Macromolecules

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

https://doi.org/10.1016/j.ijbiomac.2024.132410

Received 13 January 2024; Received in revised form 4 May 2024; Accepted 13 May 2024

International Journal of Biological Macromolecules xxx (xxxx) xxx

cycling during the formation of RS could modify its recrystallization,

thereby inuencing the structural stability and formation of RS. In our

previous work, we focused on evaluating the structure and properties of

RS obtained using various methods, and discovered that autoclaving-

microwave combination was conducive to RS formation [17]. Howev-

er, the effect of retrogradation conditions on the formation of RS in this

process has not been explored. In this study, the impact of retrograda-

tion temperature conditions following autoclaving-microwave process-

ing on the structural characteristics and digestibility of starch during the

formation of RS3 was meticulously investigated. This research provides

a theoretical foundation for efciently managing the retrogradation

process after autoclave-microwave treatment, which hope to facilitate

the production of healthy functional ingredients with a high RS content.

2. Materials and methods

2.1. Materials

Normal maize starch (NM, Apparent amylose content (AAC) =26.82

%) was obtained from Qinhuangdao Lihua Starch Co., Ltd. (Qinhuang-

dao, China). Hylon VII (HAM, AAC =72.39 %) was purchased from the

Ingredion Incorporated (Westchester, USA). Porcine pancreatic a-

amylase and glucoamylase (300 U/mL) were obtained from Sigma-

Aldrich (St. Louis, MO, USA) and Shanghai Yuanye Bio-Technology

Co., Ltd. (Shanghai, China), respectively. Other reagents were analyt-

ical grade and purchased from domestic reagent companies.

2.2. Sample preparation

A constant temperature oscillator (100 ◦C) (SHA-B, Guangzhou

Guohua Electric Appliance Co., Ltd.) was used to pre-gelatinize 7.5 g of

HAM or NM in 50 mL of deionized water for 15 min. The pregelatinized

starch was sealed within a polyethylene lm to minimize moisture loss,

and subsequently autoclaved (121 ◦C, 0.1 MPa) in a high-pressure steam

sterilizer (ZM-100, Guangzhou Biaoji Packaging Equipment Co., Ltd) for

30 min. Subsequently, the sample was immediately subjected to mi-

crowave heating using a microwave power dose (MKJ-J1–3, Nanjing

Heben Microwave Technology Development Co.) of 12 W/g of starch

slurry for a duration of 3 min. The sample was allowed to cool naturally

to room temperature before being stored at 4 ◦C for 24 h. Subsequently,

the sample was divided into 6 groups. The design of the temperature

cycle conditions is based on the research by Zeng et al. [18], with slight

modications. Each group was transferred and stored separately at one

of the following temperatures: 4 ◦C, 10 ◦C, 20 ◦C, 30 ◦C, 40 ◦C, or 50 ◦C

for 24 h. This operation was repeated 4 times to obtain retrograded

starch samples. The end products were quickly freeze-dried using a

vacuum freeze dryer (FD-1-50, Beijing Bo Yikang Experimental Instru-

ment Co., Ltd.), ground into powders, and passed through a 100-mesh

sieve for further analyses. Based on the retrogradation conditions, the

HAM samples were named HAM-4, HAM-4-10, HAM-4-20, HAM-4-30,

HAM-4-40, and HAM-4-50. Similarly, the NM samples were named NM-

4, NM-4-10, NM-4-20, NM-4-30, NM-4-40, and NM-4-50, respectively.

2.3. Short-range ordered structure

2.3.1. Fourier transform infrared (FTIR) spectroscopy

The sample preparation was determined according to the method

described by Zhang et al. [19]. Each sample was placed in an FTIR

spectrometer (Nexus 470, Thermo Nicolet, Inc., Wisconsin, USA) and

scanned 64 times at a resolution of 4 cm

−1

over a wavelength range of

4000–400 cm

−1

. Each sample was scanned 3 times, and the spectrum

was analyzed by the Omnic 8.2 software.

2.3.2. Raman spectroscopy

The raman spectra of all samples were obtained using a raman

spectrometer (Nexus, Thermo Nicolet, Inc., Wisconsin, USA). The laser

source, laser power, spectral resolution, spectral measurement range,

and number of scans were Nd: YAG (λNd: YAG =1064 nm), 1 W, 8 cm

−1

300–3500 nm, and 500 times, respectively. The analysis of the spectra

and the calculation of the half-width height of the corresponding char-

acteristic peaks were conducted by the Omnic 8.2 software and Peakt

software, respectively.

2.4. X-ray diffraction (XRD)

The crystallization characteristics of specimens were determined

using a powder X-ray diffractometer (D8 Advance; Bruker, Karlsruhe,

Germany) at 40 kV and 40 mA according to the previous research [9].

The samples were scanned at a speed of 2◦/min in the diffraction angle

(2θ) range of 3 to 35◦with a step of 0.02◦. The relative crystallinity (RC)

was analyzed using Peakt and Jade 6.5 and calculated according to the

following equation [20]:

RC =Ac

Ac +Aa⨯100%

Ac: The area of the crystalline region; Aa: The area of the amorphous

region.

2.5.

C CP/MAS NMR

The Varian Innity-plus 400 MHz was used to complete

C CP/MAS

NMR studies. Measurement parameters: a solid-state 4 mm detection

probe, a 400 MHz NMR intensity, a 38 KHz spectral width, a 3 ms sample

contact time, a 50 ms data collection time, and a minimum of 3000 scans

were utilized. In accordance with Tan et al. [21], the data were analyzed

using the Excel Solver data analysis tool and the Peakt software.

2.6. Aqueous leaching (AML) and swelling power

Swelling power was determined by referring to the method described

by TESTER et al. [22] with slight revisions. Fifty milligrams (W) of

starch suspension were incubated (10 mg/mL) at 55, 60, 65, 75, 85, and

95 ◦C for 30 min in tubes. The tubes were cooled to room temperature

before 0.5 mL of blue dextran (Mr =2 ×10

g/mol, 5 mg/mL) was

added and mixed. The absorbance of the supernatant (AS) after centri-

fugation (1500 g, 5 min) and the absorbance of the reference tube

without starch (AR) were nally measured at 620 nm. The calculation of

the swelling factor (SF) was based on the following equation [22]:

SF =1+ {(7700/W) [(As −AR)/As ] }

The leaching efciency of amylose was determined according to the

method described by Watcharatewinkul et al. [23] with minor modi-

cations. A suspension of 200 mg of starch (dry weight basis) in 10 mL of

distilled water was sealed and incubated for 30 min at each of the

following temperatures: 55 ◦C, 60 ◦C, 65 ◦C, 75 ◦C, 85 ◦C, and 95 ◦C.

They were cooled to room temperature and centrifuged (2000 g) for 10

min. The amylose content of 1 mL of the supernatant was measured

[24]. Amylose leaching (AML) was calculated as the percentage of

amylose content precipitated from 100 g of dry starch.

2.7. In vitro digestibility

2.7.1. In vitro simulated digestion experiments

The previously described methods were modied to simulate diges-

tion experiments in vitro [25,26]. Briey, 200 mg of starch was dispersed

in 15 mL of sodium acetate buffer (0.1 mol/L, pH =5.2) and incubated

at 37 ◦C for 5 min. Subsequently, 10 glass beads and 5 mL of mixed

enzyme solution were added. The preparation of the mixed enzyme

solution involved the following steps. 12 mg of porcine pancreatic a-

amylase was added to a beaker containing 80 mL of deionized water and

stirred for 10 min. The mixture was then centrifuged at 1500 g for 10

J. Jiang et al.

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Comparison of structural and in vitro digestive properties of autoclave-microwave treated maize starch under different retrogradation temperature conditions

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