Oral soluble shell prepared from OSA starch incorporated with tea polyphenols for the microencapsulation of Sichuan pepper oleoresin: Characterization, flavor stability, release mechanisms and its application in mooncake

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Food Chemistry 451 (2024) 139478

Available online 25 April 2024

Oral soluble shell prepared from OSA starch incorporated with tea

polyphenols for the microencapsulation of Sichuan pepper oleoresin:

Characterization, avor stability, release mechanisms and its application

in mooncake

Jiong Zhang

, Min Zhang

, Yuchuan Wang

, Bhesh Bhandari

, Mingqi Wang

State Key Laboratory of Food Science and Resources, Jiangnan University, 214122 Wuxi, Jiangsu, China

Jiangsu Province International Joint Laboratory on Fresh Food Smart Processing and Quality Monitoring, Jiangnan University, 214122 Wuxi, Jiangsu, China

School of Agriculture and Food Sciences, University of Queensland, Brisbane, QLD, Australia

Zhengzhou Xuemailong Food Flavor Co. R&D Center, Zhengzhou, Henan, China

ARTICLE INFO

Keywords:

Sichuan pepper oleoresin

Microencapsulation

Flavor stability

Release mechanism

Mooncake avor enhancement

ABSTRACT

The market share of Sichuan pepper oleoresin (SPO) in the avor industry is increasing steadily; however, its

high volatility, low water solubility, and poor stability continue to pose signicant challenges to application. The

microencapsulation prepared by emulsion embedding and spray drying is considered as an effective technique to

solve the above problems. Sodium octenyl succinate starch (OSA starch) and tea polyphenols (TPs) were used to

develop OSA-TPs complex as encapsulants for SPO to prepare orally soluble microcapsules. And the optimum

doping of TPs was determined. SPO microcapsules have good properties with high encapsulation efciency up to

88.13 ±1.48% and high payload up to 41.58 ±1.86% with low water content and high heat resistance. The

binding mechanism of OSA starch with TPs and its regulation mechanism and effect on SPOs were further

analyzed and claried. The binding mechanism between OSA starch and TPs was claried in further analyses.

The OSA-TPs complexes enhanced the rehydration, release in food matrix and storage stability of SPO, and

exhibited good sensory immediacy. Flavor-improved mooncakes were successfully developed, achieving the

combination of mooncake avor and SPO avor. This study provided a valuable way to prepare avoring mi-

crocapsules suitable for the catering industry, opened up the combined application of SPO and bakery in-

gredients, and was of great practical value and signicance for improving the processing quality of avor foods,

driving the development of the SPO industry, and enhancing the national dietary experience.

1. Introduction

Sichuan pepper (Zanthoxylum bungeanum) is one of the traditional

spices widely cultivated and consumed around the world and is often

used as the avor enhancer in the form of direct use. With further

research, Sichuan pepper essential oil (SPEO) and Sichuan pepper

oleoresin (SPO) extracted from Sichuan pepper with typical pepper

avor are also the mainstream products in the current seasoning market.

The difference is that SPO contains not only SPEO, but also highly

concentrates the non-volatile avor components (Zhang et al., 2022).

SPO provides more intense aroma and fuller avor in a smaller amount

than Sichuan pepper and SPEO. As a result, SPO is gradually achieving to

replace them in the home cooking and food processing industries as a

popular ingredient in products such as hotpot base, baking, small crispy

meats and Sichuan sausages. However, low water solubility and the

instabilities such as high volatility and susceptibility to oxidation and

decomposition by light, heat and oxygen limit its more widespread use.

Currently, emulsions and microencapsulation are common means to

improve the defects and applicability of SPO. In contrast, microcapsules

not only provide better protection than emulsions, but are also easier to

use, store and transport. And, it would make more sense to apply SPO in

powder form in specic scenarios.

Microencapsulation is the capture of core material into a polymer

wall material that is easily lm-forming to prevent the loss of core

substance and improve its water solubility and dispersibility (Zhao et al.,

2023). Also, microencapsulation enables controlled and targeted release

* Corresponding author at: State Key Laboratory of Food Science and Technology, Jiangnan University, 214122 Wuxi, Jiangsu, China.

E-mail address: min@jiangnan.edu.cn (M. Zhang).

Contents lists available at ScienceDirect

Food Chemistry

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

https://doi.org/10.1016/j.foodchem.2024.139478

Received 4 January 2024; Received in revised form 4 April 2024; Accepted 23 April 2024

Food Chemistry 451 (2024) 139478

of the core material. Microencapsulated foods continue to push the

boundaries and have been involved in many applications such as bev-

erages, solid yoghurt, meat products, dairy products and many others

(Calderon-Oliver & Ponce-Alquicira, 2022; Huang, Liang, Sun, Brennan,

& Liu, 2021; Su et al., 2023). In recent years, researches involved in SPO

microcapsules have mainly focused on the development of novel carriers

and the further utilization of bioactivities, while research on combining

them with practical application scenarios to develop specialty avored

foods for catering is lacking (Chen, Zhang, Adhikari, & Wang, 2022;

Procopio, Ferraz, Paulino, do Amaral Sobral, & Hubinger, 2022). And

thermal processing is usually unavoidable in this process. In addition, if

the unique avor of the internal SPO is not quickly perceived by the

body due to the wrapping of the wall material, it will reduce the interest

of the consumers.

Therefore, taking into account the heat resistance as well as the

releasability of the microcapsules, we chose orally digestible sodium

octenyl succinate starch (OSA starch) as the wall material to powder

SPO. As we all know, OSA starch has the advantages of wide source, high

safety, strong emulsifying ability and good microencapsulation effect

(Lin, Liang, Zhong, Ye, & Singh, 2018), which can avoid the safety

problems caused by adding surfactants and easy caking of microcapsules

when used as food emulsier and encapsulation material. From previous

reports, it was found that when OSA starch was used as encapsulated

material for preparing microcapsules by spray drying, it was also usually

combined with drying aids in the system to form multiple layers of walls

to provide additional stability. The multilayer wall system refers to the

stepwise mixing of multiple wall materials together to form a co-

encapsulation. For example, Fang, Zhao, Liu, Liang, and Yang (2019)

used OSA starch and chitosan to prepare multilayer emulsions suitable

for spray drying to encapsulate β-carotene. De Barros Fernandes, Borges,

and Botrel (2014) selected the binary system consisting of modied

starch and maltodextrin to encapsulate rosemary essential oil, which

showed high encapsulation and retention of microcapsules after spray

drying. Also, microcapsules constructed with OSA starch, whey protein

isolate and inulin as substrates exhibited signicant thermal stability

and up to 87% loading of diacylglycerol oil as reported by Guo, Fan,

Zhou, and Li (2023). However, the multiple wall materials are detri-

mental to the release of active ingredients. And when only OSA starch

was used as the Pickering emulsion, the oil phase in the emulsion was

susceptible to oxidation due to the large oil-water interface, so the single

OSA starch as encapsulant did not provide good protection for oxidiz-

able condiments during the spray drying stage (Wang & Zhou, 2022).

Tea polyphenols (TPs) are naturally non-toxic polyphenolic com-

pounds recognized for their strong antioxidant activity as well as heat

resistance and are widely used in food systems. It was reported that the

combination of TPs with emulsiers at the emulsion interface protected

the oil phase from oxidation. And, hydrogen bonding between raw

starch and phenolic compounds has been demonstrated (Li, Ndiaye,

Corbin, Foegeding, & Ferruzzi, 2020).

Based on this, in this study, OSA starch and TPs were purposely

selected as raw materials to construct the monolayer wall for encapsu-

lation of SPO with OSA starch-TPs complexes as the main body, followed

by spray-dry granulation. Subsequently, the mechanism and effect of

TPs incorporation on the regulation of the microcapsule system and the

performance advantages of SPO microcapsules with OSA-TPs complexes

as the wall material were investigated through the characterization of

the basic properties, thermal stability, structural features, volatility

stability, release behavior and storage stability of the prepared micro-

capsules. Finally, the microcapsules were used for avor improvement

in bakery mooncakes, aiming to provide a valuable route for the prep-

aration of avor microcapsules suitable for the catering industry.

2. Materials and methods

2.1. Materials and reagents

Sichuan pepper oleoresin (SPO), which was obtained by supercritical

of red Sichuan pepper from Wudu, Gansu, China, was supplied by

Zhengzhou Xuemailong Food & Spice Co., Ltd. (Henan, China). Sodium

octenyl succinate starch (ORS4, Degree of substitution: 1.25) from

Foshan Summit Starch Technology Co., Ltd. (Guangdong, China) was

formed by hydrophobically modifying waxy corn starch. Tea Poly-

phenols (>98%, containing 40% EGCG) was bought from Xi'an Tian-

guangyuan Biotechnology Co., Ltd. (Shanxi, China).

Ethanol (>99.7%) and acetic acid (CH

COOH, >99.5%) were all

bought from Sinopharm Chemical Reagent Co., Ltd. (Shanghai, China).

Trichloromethane was distributed by Jiangnan University Experimental

Materials Warehouse.

2.2. Preparation of SPO-loaded emulsions and microcapsules

The emulsions were prepared with reference to Li et al. (2023) and Li

et al. (2023) with minor modications. In a nutshell, OSA starch and TPs

were dissolved in deionized water to obtain OSA starch solution (1%, w/

w) and TPs solution (0.1%, 0.3%, 0.5%, w/w), respectively. The TPs

solution was dropped into the OSA starch solution under magnetic

stirring and stirred at 600 rpm overnight at room temperature to allow

for adequate hydration and incubation. The fresh liquid was freeze-dried

to obtain OSA starch-TPs complex. Afterwards, the complex solution

(1%, w/w) containing different concentrations of TPs prepared using

deionized water was heated at 65 ◦C for 20 min. After cooling, SPO was

added to it in the ratio of 1:1. The mixing systems were treated with the

high-speed shear disperser (IKA®-T18 basic, Shanghai Ziqi Experi-

mental Equipment Co., Ltd., China) at 10,000 rpm for 3 min and then

homogenized by the high-pressure homogenizer (JHG-54-P100,

Shanghai Pricerite Fusion Machinery Co., Ltd., China) at 30 MPa for 2

cycles to obtain the nal emulsions. The nal emulsions were named

OSA, OSA-10% TPs, OSA-30% TPs, and OSA-50% TPs.

The nal emulsions were spray dried (B-290, BUCHI Labortechnik

AG, Switzerland) to produce powders that were SPO microcapsules,

named OSA microcapsules, OSA-10% TPs microcapsules, OSA-30% TPs

microcapsules and OSA-50% TPs microcapsules, respectively. Working

parameter setting: temperature of air inlet and outlet: 165 ◦C and 85 ◦C;

feed rate: 15 mL/min; air pressure: 0.4 MPa; aspirator: 85%. Emulsions

and microcapsules were stored at 4 ◦C for subsequent testing.

2.3. Characterization of SPO emulsions

2.3.1. Measurement of droplet size and zeta potential

The average size and size distribution of the droplets of prepared

emulsions containing different concentrations of TPs were measured by

the nano particle size and zeta potential meter (Zetasizer nano ZS,

Malvern Instruments Ltd., UK).

2.3.2. Measurement of interfacial tension

The oil-water phase interfacial tension of the above four emulsions

was determined using the fully automatic surface tension meter

(DCAT21, DFE Chemicals Co., Ltd., Stuttgart, Germany).

2.4. Determination of basic properties of SPO microcapsules

2.4.1. Encapsulation efciency and payload

The content of surface oil (SO) and total oil (TO) of SPO microcap-

sules was measured to determine the encapsulation efciency and

payload, as follows.

SO: the claried liquid collected was the trichloromethane solution

containing SO when 0.5 g of SPO microcapsules were dispersed in a

sample bottle containing 20 mL trichloromethane and ltered after

J. Zhang et al.

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