Preparation, structural and functional characterization of corn peptide-chelated calcium microcapsules using synchronous dual frequency ultrasound

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Ultrasonics Sonochemistry 102 (2024) 106732

Available online 19 December 2023

nc-nd/4.0/).

Preparation, structural and functional characterization of corn

peptide-chelated calcium microcapsules using synchronous dual

frequency ultrasound

Wenjuan Qu

, Yuhang Feng

, Ting Xiong

, Abdul Qayum

, Haile Ma

School of Food and Biological Engineering, Jiangsu University, Zhenjiang 212013, China

Institute of Food Physical Processing, Jiangsu University, Zhenjiang 212013, China

ARTICLE INFO

Keywords:

Corn peptide-chelated calcium

Microcapsule

Dual-frequency ultrasound

Structural characterization

Stability

Solubility

ABSTRACT

The utilization of peptide-chelated calcium is low due to the inuence of factors such as solubility, heat and

digestive environmental conditions; therefore, it is crucial to protect, prolong and stabilize this nutrient in order

to enhance its efcacy. This study was conducted to prepare corn peptide-chelated calcium microcapsules using

β-cyclodextrin (β-CD) as the wall material through an improved ultrasonic-assisted method. The structure, sol-

ubility, thermal stability, and in vitro gastrointestinal digestion of these microcapsules were thoroughly inves-

tigated and analyzed. The microcapsules were prepared using the following recommended conditions: a chelate

concentration of 5 mg/mL, a mass ratio of chelate to β-CD of 1:8 g/g, and a synchronous dual-frequency ul-

trasound (20/28 kHz) at a power of 75 W, a duty ratio of 20/5 s/s, and a time of 20 min. These specic pa-

rameters were carefully selected to ensure the optimal fabrication of the microcapsules. The results showed that

the utilization of dual-frequency ultrasound resulted in a signicant increase in both the encapsulation rate and

yield, which were enhanced by 15.84 % and 15.68 %, respectively, reaching impressive values of 79.17 % and

90.60 %. Moreover, the results of the structure index analysis provided further conrmation that ultrasonic

treatment had a signicant impact on the structure of the microcapsules, leading to a noticeable reduction in

particle size and transformation into nanoparticles. Furthermore, the microcapsules demonstrated excellent

solubility within a wide pH range of 2 to 10, with solubility ranging from 93.54 % to 88.68 %. Additionally, these

microcapsules exhibited remarkable thermal stability, retaining a minimum of 84.8 % of their stability when

exposed to temperatures ranging from 40 to 80 ◦C. Moreover, during gastric and intestinal digestion, these

microcapsules exhibited a high slow-release rate of 44.66 % and 51.6 %, indicating their ability to gradually

release calcium contents. The inclusion of dual-frequency ultrasound in the preparation of high calcium mi-

crocapsules yielded promising outcomes. Overall, our work presents a novel method for synthesizing corn

peptide-chelated calcium microcapsules with desirable properties such as good solubility, excellent thermal

stability, and a signicant slow-release effect. These microcapsules have the potential to serve as fortied high

calcium supplements.

1. Introduction

Recent studies have revealed that peptide-chelated calcium, a novel

fortied high calcium supplement, exhibits enhanced safety and a

higher calcium content when compared to commonly used calcium

supplements such as amino acid calcium, organic calcium salts, and

inorganic calcium salts [1–4]. However, when ingested directly in the

body, peptide-chelated calcium exhibits low bioavailability due to its

low solubility and susceptibility to degradation under high temperature

and gastrointestinal digestion conditions. Furthermore, the bitter taste

associated with peptides also poses a limitation on the application of

peptide-chelated calcium [5], affecting the overall taste of the product.

Hence, the design of a valuable formulation to enhance the solubility,

thermal stability, and slow-release effect of peptide-chelated calcium

becomes crucial in addressing these limitations effectively.

Microcapsule embedding technology provides a promising approach

to protect products by encapsulating them within a stable natural or

synthetic wall material, effectively addressing the aforementioned

* Corresponding author at: School of Food and Biological Engineering, Jiangsu University, 301 Xuefu Road, Zhenjiang 212013, China.

E-mail address: wqu@ujs.edu.cn (W. Qu).

Contents lists available at ScienceDirect

Ultrasonics Sonochemistry

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

https://doi.org/10.1016/j.ultsonch.2023.106732

Received 14 November 2023; Received in revised form 3 December 2023; Accepted 14 December 2023

Ultrasonics Sonochemistry 102 (2024) 106732

challenges. A commonly utilized wall material in this context is

β-cyclodextrin (β-CD), owing to its external hydrophilic and internal

hydrophobic characteristics. The hydrophobic groups of the products

can stably bind with the interior of β-CD, resulting in a favorable

embedding effect [6–9]. It has been reported that thymol can form an

inclusion complex with β-cyclodextrin to enhance its water solubility

and thermodynamic stability based on the preservation of its own bio-

logical activity [6]. In addition, ultrasonic technology has been shown to

be effective in creating encapsulated materials with specic physical and

functional properties, due to its cavitation and mechanical effects

[10–13]. This is attributed to the wide range of active frequencies of

ultrasound, enabling precise control over the intensity and frequency of

cavitation events, which in turn can be utilized to manipulate material

properties such as particle size, surface roughness, and structure [11].

Consequently, this technique has the potential to enhance the functional

properties of materials. Sun et al. [13] reported that ultrasound can

improve the solubility and thermal stability of the inclusion complex of

thymol with 2-hydroxypropyl-β-cyclodextrin by improving the complex

structure and increasing the molecular interactions, such as hydrogen

bonding and hydrophobic interactions. Hence, a promising strategy to

produce peptide-chelated calcium microcapsules exhibiting enhanced

solubility, thermal stability, and controlled release is suggested by

combining encapsulation and ultrasonic technology. Currently, the most

common ultrasonic encapsulation is single-frequency ultrasonic device.

There is extensive evidence that synchronous dual-frequency sonication

signicantly increases mechanical disturbance and cavitation yield

compared to a single-frequency ultrasound, due to the stronger intensity

of the ultrasonic eld generated by the superposition of the two fre-

quencies, the lower cavitation threshold and the enhanced nucleation

and collapse of bubbles [14,15]. Chen et al. [16] found that dual-

frequency ultrasound generated a greater number of cavitation bub-

bles and exhibited a stronger cavitation effect on Qingke protein

compared to single-frequency ultrasound. However, there is currently a

lack of research and scientic reports exploring the application of ul-

trasonic technology, specically advanced dual-frequency ultrasound,

in the production of peptide-chelated calcium microcapsules. Therefore,

the core aim of this study was to employ the synchronous dual-frequency

ultrasonic enhancement technique to fabricate corn peptide-chelated

calcium microcapsules encapsulated with β-CD. The innovative aspect

of our study is focused on determining the encapsulation rate and yield,

as well as exploring the effects of encapsulation and ultrasound tech-

niques on the structure, solubility, thermal stability, and slow-release

properties of the microcapsules. These ndings aim to evaluate the po-

tential of the microcapsules as a promising alternative for high calcium

supplementation.

2. Materials and methods

2.1. Materials

Corn gluten meal was obtained from Jiahui Feed Enterprise (Hebei,

China). Neutrase and Alcalase (the activity of 50 U/mg and 269 U/mg,

respectively) were purchased from Novozymes Co., ltd. (Jiangsu,

China). Pepsin and trypsin (the activity of 3000 U/mg and 250 U/mg,

respectively) were purchased from Sigma Company (St. Louis, MO,

USA). β-CD, ethylenedinitrilotetraacetic acid (EDTA) and other analyt-

ical grade chemicals were purchased from Sinopharm Chemical Reagent

Co. Ltd (Shanghai, China).

Corn peptide was prepared following the procedure outlined in our

previous publication [4]. Corn gluten meal solution (80 mg/mL) was

hydrolyzed using Neutrase at an enzyme-substrate ratio of 2000 U/g, pH

7, 50 ◦C for 2.5 h. The resulting solution was then subjected to ultra-

ltration purication (using a 30 kDa membrane), to obtain the corn

permeates (10.86 mg/mL, 1.5 L). These permeates were subsequently

hydrolyzed further using Alcalase at an enzyme-substrate ratio of 8000

U/g, pH 8.5, and 40 ◦C for 5 h. The hydrolysis process was performed

using synchronous dual-frequency ultrasound (20/28 kHz) at a power of

225 W, a duty ratio of 10/5 s/s, and four cycles (with a work-time of 40

min and a stop-time of 20 min). After another round of ultraltration

purication (using a 3 kDa membrane) and dialysis (with a size cutoff of

100 Da), the resulting solution was obtained as the corn peptide

solution.

2.2. Preparing corn peptide chelated calcium microcapsules using

ultrasonication method

Corn peptide-chelated calcium was prepared according to our pre-

vious publication [4]. The CaCl

was added to the corn peptide solution

(36 mg/mL, 15 mL) at a mass ratio of 1:8 g/g, pH 7, 40 ◦C for a chelating

time of 40 min. The reaction solution was then mixed with eight times

the volume of absolute ethanol to precipitate the chelate for 60 min at

25 ◦C. The chelate precipitates were removed from ethanol-soluble non-

chelated calcium and peptides by centrifugation at 4000×g for 15 min,

collected, and then freeze-dried. The freeze-dried chelate was

completely dissolved in distilled water and mixed with the β-CD aqueous

solution using the synchronous dual-frequency (20/28 kHz) ultrasound

for a total embedding time of 30 min to ensure complete embedding. The

microcapsule supernatant was collected after centrifugation (4000×g

for 15 min), and then freeze-dried. The effects of chelate concentration

(1, 2.5, 5, 7.5, 10 mg/mL), mass ratio of chelate to β-CD (1:2, 1:4, 1:6,

1:8, 1:10 g/g), ultrasonic power (6, 25, 50, 75, 100 W), duty ratio (10/5,

20/5, 30/5, 50/5 s/s), and time (5, 10, 15, 20, 30 min) on the encap-

sulation rate of chelate and the yield of microcapsules were studied to

investigate the effects of various parameters on the preparation of

microcapsules.

2.3. Encapsulation rate and yield measurements

The encapsulation rate was determined according to the method of

Chen et al. [17] with some modications. Freeze-dried microcapsules

(50 mg) were dissolved uniformly in absolute ethanol (25 mL). The

ethanol-insoluble precipitates (i.e. unmicroencapsulated chelates) were

removed from the ethanol-soluble microcapsules by centrifugation at

4000×g for 15 min, collected and then freeze-dried. The dried unmi-

croencapsulated chelate was completely dissolved in distilled water and

the calcium content was measured by the EDTA titration method ac-

cording to our previous publication [4]. The encapsulation rate and the

yield were calculated using Equations (1) and (2):

Encapsulation rate(%) = (1−m

′

) × 100 (1)

Yield (%) = m0

′

3+m

′

×100 (2)

where, m

′

is the initial calcium content in the sample (mg), m

′

is the

calcium content in the unmicroencapsulated chelate (mg), m

is the dry

mass of microcapsules (mg), m

′

is the dry mass of chelate (mg), and m

′

is the dry mass of β-CD (mg).

2.4. Fourier transform infrared (FTIR) spectroscopy

The chelate, β-CD, and microcapsules were mixed with dry potas-

sium bromide in a mass ratio of 1:100, uniformly ground, and pressed

into 1–2 mm akes. The ake was loaded on the FTIR spectrograph

(Thermo Fisher Scientic Corporation, USA). The spectra of the samples

were recorded with a scan range of 4000–500 cm

−1

by 32 scans at a

resolution of 4 cm

−1

W. Qu et al.

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