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Food Research International 151 (2022) 110879

Contents lists available at ScienceDirect

Food Research International


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

Review

Current trends in flavor encapsulation: A comprehensive review of


emerging encapsulation techniques, flavour release, and
mathematical modelling
Yashaswini Premjit a, Shikha Pandhi b, *, Arvind Kumar b, Dinesh Chandra Rai b,
Raj Kumar Duary b, Dipendra Kumar Mahato c
a
Agricultural & Food Engineering Department, Indian Institute of Technology Kharagpur, Kharagpur 721302, West Bengal, India
b
Department of Dairy Science and Food Technology, Institute of Agricultural Sciences, Banaras Hindu University, Varanasi 221005, Uttar Pradesh, India
c
CASS Food Research Centre, School of Exercise and Nutrition Sciences, Deakin University, Burwood, VIC 3125, Australia

A R T I C L E I N F O A B S T R A C T

Keywords: Food flavors are volatile compounds that impact the human sensory perception profoundly and find extensive
Flavor release applications in various food products. Because of their volatility and high sensitivity to pH, temperature,
Microencapsulation oxidation, and external conditions, they require adequate protection to last for a longer duration. Encapsulation
Nanoencapsulation
plays a critical role in preserving food flavors by enhancing their thermal and oxidative stability, overcoming
Controlled release
Kinetic modelling
volatility limitations, and regulating their rapid release with improved bioavailability in food products. The
current review focuses on the recent developments in food flavor encapsulation techniques, such as electro­
spinning/spraying, cyclodextrin inclusion complexes, coacervation, and yeast cell micro-carriers. The review also
comprehensively discusses the role of encapsulants in achieving controlled flavor release, the mechanisms
involved, and the mathematical modelling for flavor release. Specific well-established nanoencapsulation tech­
niques render better encapsulation efficiency and controlled release of flavor compounds. The review examined
specific emerging methods for flavor encapsulation, such as yeast cell encapsulation, which require further
exploration and development. This article provides readers with up-to-date information on different encapsu­
lation processes and coating methods used for flavor encapsulation.

1. Introduction approaches for increasing flavor stability and reducing degradation. It


protects flavoring compounds from oxidative and thermal degradation
Flavoring agents are volatile organic compounds widely used as during processing (Feng et al., 2018). An active ingredient is encapsu­
crucial components in the beverage, savory, snack, confectionery, frozen lated within a wall material/coating material/encapsulant that protects
products, and dairy industries (Saffarionpour, 2019). These compounds it from deteriorative conditions (Ocampo-Salinas et al., 2020). This
profoundly affect the human sensory perception and influence the creates a protective layer around the flavor droplet, allowing it to be
product acceptability among consumers (Sultana et al., 2018). However, covered while masking unpleasant taste (Saifullah et al., 2019).
since most flavors are volatile liquids that evaporate and degrade Encapsulation also improves the product functionality by allowing
quickly, it is critical to protect them from harsh environmental condi­ variable properties (particle size, structure, and shape), easier handling,
tions and undesirable ingredient interactions during storage and pro­ and controlled or triggered flavor release under predetermined condi­
cessing (Kim et al., 2019a). Food processors are concerned about flavor tions (Kim et al., 2019a).
stability at an acceptable degree of power. Moreover, flavors are Microencapsulation and nanoencapsulation are the two most popu­
extremely sensitive to pH, moisture, acid, salt, and enzyme action, lar techniques of generating particles with diameters ranging from a few
which can cause off-flavors (Feng et al., 2018; Fuciños et al., 2017; nanometers to a few millimeters. These methods offer improved product
Saifullah et al., 2019). functionality by masking unpleasant flavors, increasing bioavailability,
Encapsulation is one of the most efficient and widely employed improving encapsulation efficiency, loading capability, and longevity,

* Corresponding author.
E-mail address: shikhapandhi94@gmail.com (S. Pandhi).

https://doi.org/10.1016/j.foodres.2021.110879
Received 21 May 2021; Received in revised form 29 November 2021; Accepted 4 December 2021
Available online 9 December 2021
0963-9969/© 2021 Elsevier Ltd. All rights reserved.
Y. Premjit et al. Food Research International 151 (2022) 110879

and achieving a sustained release profile. A variety of encapsulating difficulties of encapsulating flavors (Khanum et al., 2018):
materials and encapsulation techniques are required to develop suitable 1. Flavoring compounds are primarily available as liquids.
flavor encapsulation systems (Samakradhamrongthai et al., 2019). 2. Flavors are a mixture of different components with varying
Spray drying (SD), fluidization bed coating, spray cooling/chilling, and physicochemical properties.
extrusion are mechanical microencapsulation techniques, while molec­ 3. Flavors possess varying sensory thresholds.
ular inclusion, interfacial polymerization, coacervation, and co- 4. Flavors have single release kinetics in most cases.
crystallization are chemical microencapsulation techniques (Saini 5. Flavors may react with specific food ingredients under certain
et al., 2020). conditions.
Nanoscale delivery systems have piqued a much greater interest than 6. In a water-continuous environment, flavor stabilization is difficult.
microencapsulation techniques because of their superior functional
properties, such as increased encapsulation efficiency, controlled 3. Role of encapsulants/coating materials
release, improved stability, , and increased bioavailability of in­
gredients. Nanocarriers are further classified into lipid-based nano­ The choice of encapsulants, which play an essential role in the
carriers (nanoemulsions, nanolipid carriers), nature-inspired encapsulation, safety, and long-term release of biomolecules, could be a
nanocarriers (caseins, cyclodextrins, amylose), special equipment-based promising solution for nutraceutical formulations. Encapsulants must
nanocarriers (electrospinning/electrospraying, nanospray dryer, possess specific characteristics, such as being food-grade, having a
micro-/nanofluidics), and biopolymer-based nanocarriers (single Generally Recognized as Safe (GRAS) status, being compatible with
biopolymer nanoparticles, complex biopolymer nanoparticle, nanogels, other food matrix ingredients, having a high payload, and providing
nanotubes/nanofibrils) (Saini et al., 2020). substantial safety from degradation (Kumar et al., 2018; Pandhi et al.,
The controlled release method for encapsulated compounds has the 2021).
advantage of releasing active compounds at a steady rate over time
while also minimizing ingredient losses during cooking and processing. 3.1. Carbohydrate-based encapsulants
Several studies have been conducted to investigate the flavor release
activity from encapsulated matrices. Diffusion, swelling, melting, and Carbohydrates are popular carriers for many bioactive substances
decay are four common ways by which the release occurs . The encap­ because of their biocompatibility, biodegradability, structural flexi­
sulated system stability and release properties are greatly influenced by bility, and site digestion properties. They outperform lipids and proteins
the choice of the wall material and storage conditions (Sultana et al., in terms of thermal stability, availability, and the ability to encapsulate
2018). hydrophilic and hydrophobic compounds. Unlike proteins responsible
In the present-day context, there is an exceptional interest in for colloidal aggregation and flocculation, they are less sensitive to
encapsulating flavoring agents and several studies have been conducted environmental changes (particularly pH and ionic strength) (Fathi et al.,
to improve and build on existing micro- and nanoencapsulation tech­ 2021). The four main groups of carbohydrate-based delivery systems are
niques in the past couple of years. Therefore, this review aims to plant origin (starch, gum Arabic, guar gum, pectin), animal origin
exhaustively compile the latest research and explore the advances in (chitin, chitosan), algal origin (agar, carrageenan, alginate), and mi­
food flavor encapsulation, emphasizing micro- and nano-encapsulation crobial origin (xanthan gum, dextran, cyclodextrin) (Kumar et al.,
processes, encapsulating materials, and their related release mecha­ 2018).
nisms. Novel and emerging techniques, including electrospinning/ Chitosan is a hydrophilic, linear polysaccharide that increases the
spraying, cyclodextrin inclusion complexes, coacervation, and yeast cell bioavailability of bioactive compounds by extending the residence time
microcarriers, have been detailed in the article. We also comprehen­ of the delivery system in the gastrointestinal tract. Other widely used
sively discuss the role of encapsulants in achieving controlled flavor polysaccharide delivery systems include alginate extracted from brown
release along with the mechanisms of the process, besides mathematical seaweeds, carrageenan derived from marine algae, and xanthan gum
modelling for flavor release. While the review sheds light on certain from the microorganism, Xanthomonas campestris (de Souza Simões
popular nanoencapsulation techniques, which have rendered better et al., 2017). Zhu et al. (2018) used an ultrasonic method to microen­
encapsulation efficiency and controlled release of flavor compounds, we capsulate vanilla essential oil using various wall materials, including
also explored various emerging techniques that require further devel­ jackfruit seed starch, chitosan, and cyclodextrin. They concluded that
opment, like yeast cells for flavor encapsulation. jackfruit seed starch has immense potential as an encapsulant. Another
study by Hasanvand and Rafe (2019) identified that flax seed gum-rice
2. Characteristics of flavoring compounds and need for bran protein complex coacervates to make vanillin/-cyclodextrin in­
encapsulation clusion complex (CD-IC) microcapsules resulted in higher thermal sta­
bility and a well-regulated vanillin release.
Many volatile compounds have a distinct fragrance, making them
versatile flavoring ingredients. Owing to their high volatility and 3.2. Protein-based encapsulants
chemical instability, many of these products are easily lost during food
processing, storage, and preparation. Light, oxygen, humidity, and Several critical functional properties of proteins for encapsulation
moisture negatively impact various flavor compounds. Chemical in­ include their emulsification, foaming ability, water, and oil holding
teractions, oxidation, and volatilization can alter the sensory perception capacity, high glass transition temperature, and decreased allergenicity,
of food aromas (Jedlińska et al., 2018). At high temperatures, these among many others (Akbarbaglu et al., 2021). Some sources of plant
components are lost easily, which results in an adverse alteration in the proteins include soy proteins, zein, wheat proteins, protein from le­
taste profile and biological activity. As a result, there is growing interest gumes. Research on flavor encapsulation using the corn protein, zein, by
for identifying novel techniques to monitor the stability, preservation, Dehcheshmeh and Fathi (2019) revealed that a critical factor affecting
and release of flavors in foods (Wang et al., 2019). the loading capacity and encapsulation efficiency of the saffron extract
The most critical reason to encapsulate flavors is their flexibility and was the concentration of zein. Hasanvand and Rafe (2019) employed
preservation stability. Encapsulated flavor powders have the advantage rice bran protein (RBP), a by-product of rough rice milling of rough rice
of being less prone to contamination and microbial attacks, thereby along with flaxseed gum (FG) and β-cyclodextrin (β-CD) to encapsulate
permitting prolonged storage. Since flavors are inherently volatile, the vanillin. The study found that the flavor was entrapped physically
encapsulation process keeps them stable and allows its controlled within RBP-FG coacervate, with increased thermostability of vanillin
release (Potdar et al., 2020). The following are some of the significant against external factors.

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Some animal-based proteins as encapsulants include gelatin, milk approach include, low energy supply, high reproducibility, normaliza­
proteins like whey proteins (concentrate and isolate), caseinates, and tion of the final product in terms of particle size distribution and form,
egg proteins like albumin. Whey protein isolate (WPI), a globular pro­ and decreased process time and expense. Nevertheless, oxidation, high-
tein from cheese industries, is employed extensively as an encapsulant temperature degradation, and direct exposure of bioactive compounds
for its physicochemical and functional properties. Tavares and Noreña to hot air are technical difficulties that could hinder the application of
(2020) found that the best complex coacervate yields using WPI and this technique for susceptible compounds (de Souza Simões et al., 2017).
gum Arabic (GA) were obtained at a mass ratio of 3:1 (w/w) of WPI/GA. Various encapsulating agents and drying methods, including spray
Muhoza et al. (2019) developed multinuclear microcapsules by SD, freeze-drying, and fluid bed drying, were used to test the stability of
exploiting the complex coacervation between gelatin and pectin to encapsulated strawberry flavor microcapsules (Pellicer et al., 2019). SD
protect cinnamaldehyde. They suggested that the conformation of pectin had the lowest moisture values, followed by freeze-drying and fluidized
and gelatin significantly contributed to the overall complexation and bed drying, with freeze-drying having the highest drying yield. With SD,
properties of the cinnamaldehyde microcapsules. microphotographs revealed smooth spherical crystals, while the powder
was amorphous and irregular for freeze-drying and fluidized bed drying,
3.3. Lipid-based encapsulants respectively (Pellicer et al., 2018). Another similar study was conducted
by Kim et al. (2019) wherein peppermint flavor was encapsulated
Lipid-based nano-delivery systems are among the most successful employing SD, melt extrusion, and fluidized bed drying. The study
encapsulation systems, with unrivaled advantages over the other two established that the flavors encapsulated via spray drying possessed a
systems due to their ability to entrap materials of varying solubilities more robust overall flavor perception than the same flavor concentra­
and improve targeted delivery (Pandhi et al., 2021). Lipid-based nano­ tion encapsulated by fluidized bed drying and melt-extrusion. This is
structures can accommodate and release a broad range of bioactive proof that varying the flavor encapsulation technology, and the particle
compounds (hydrophilic, lipophilic, and amphiphilic compounds) in a size could induce a varied flavor perception. The microcapsules pro­
controlled and sustained manner, improve hydrophobic compounds’ duced in all the techniques had similar flavor loads. The ranking based
solubility and encapsulation efficiency, lower volatility, and improve on decreasing flavor intensity was SD > fluidized bed drying–small
target specificity (Assadpour and Jafari, 2019). This method can resolve (<100 µm) > fluidized bed drying–large (800–1000 µm) ~ melt extru­
physicochemical uncertainty, modulate delivery profiles, and impart sion. Specifically, the fluidized bed drying with smaller particles elicited
specific sensorial characteristics (Barroso et al., 2020). Nanoemulsions, a more robust flavor perception than larger particles.
nanoliposomes, solid lipid nanoparticles (SLNs), and nanostructure lipid
carriers (NLCs) are the four central lipid-based delivery systems used 4.2. Spray drying and spray chilling
(Kumar et al., 2018).
Nanoemulsions are colloidal dispersions of liquid droplets with Spray drying (SD) is the oldest and most commonly used microen­
diameters<100 nm. They are created by encasing bioactive ingredients capsulation process in the food industry. SD is a low-cost, scalable
in a dispersed process that is self-stabilized in a continuous step by technology that enables continuous production (Takashige et al., 2020).
surfactants/biopolymers (Pandhi et al., 2021). Nanoliposomes are It is simple to set up on an industrial scale and is less expensive than
spherical complexes made of polar lipids that come together to form a other methods. SD ensures high-quality microparticles by atomizing a
lipophilic and hydrophilic group on a single molecule. The orientation of molten liquid oil mixture or emulsion through a nozzle into a hot gas
hydrophilic heads creates the bilayer and spherical core–shell configu­ chamber, resulting in a powder of particles. The SD procedure consists of
ration of the amphiphilic liposome towards the water compartment and three steps: (i) creating an active substance dispersion or emulsion, (ii)
the alignment of lipophilic tails away from the water towards the vesi­ homogenizing the dispersion, and (iii) atomizing the resulting mixture
cle’s base (Esfanjani et al., 2018). Solid-lipid nanoparticles (SLNs) are into the drying chamber. Because of the short time exposition and
submicron emulsions generated by combining two immiscible phases in accelerated water evaporation, the core temperature remains below
the presence of an amphiphilic surfactant (Pandhi et al., 2021). 40 ◦ C despite the high temperatures widely used in this phase (Nahum
Geetanjali et al. (2020) used tween 80 as a surfactant to increase and Domb, 2021).
vanillin stability during storage and processing by mixing aloe vera Jedlińska et al. (2018) examined the physicochemical properties of
mucilage in the aqueous phase with ethyl vanillin in the oil phase.. spray-dried vanilla and raspberry aroma powder. They confirmed that
According to the stability analysis of the emulsion, the vanillin remained vanilla flavors had lower fragrance retention, while raspberry flavor
stable during the study period and was successfully absorbed into a food powder had poorer flow ability, lower bulk density, smaller particle size,
cream. In another study, researchers discovered that combining stan­ and a higher glass transition temperature (Tg). Furthermore, the pow­
dard triacylglycerol oils (corn oil and MCT oil) with citrus oils (bergamot ders obtained from the cyclone container had more moisture content
oil and sweet orange oil) by varying the mixing ratios created a more and were more active. In another study aimed at extending flavor
robust mixed oil nanoemulsion with a superior physical and electronic preservation during transportation, Kim et al. (2019b) effectively
sensory property than pure citrus oil emulsions (Yang et al., 2018). microencapsulated the caramel flavor in coffee-containing dairy drinks
Bashiri et al. (2020) studied cinnamon essential oil-loaded NLC with a using medium-chain triglyceride and maltodextrin as coating materials.
variety of liquid edible oils (corn, sesamol, sweet almond, and black seed The choice of encapsulants is a significant factor affecting the SD
oil), a solid lipid (cocoa butter), and a surfactant (Tween 80). They were process. Huang et al. (2020) reaffirmed this in a study on four different
screened for physicochemical stability for 40 days under varied pH wall materials, namely chitosan, cyclodextrin, octenyl succinate anhy­
conditions (i.e., pH of milk at 6.8 and pH of certain fruit juices at 3.8) dride, and maltodextrin, for SD encapsulation to increase the stability of
and pasteurization treatment, with almond oil-based NLC showing volatile yogurt-flavored bases. They observed that chitosan possessed
encouraging performance. the best physical properties of all the materials, with enhanced encap­
sulation strength, smooth microstructure, and more excellent water
4. Encapsulation techniques for flavor compounds solubility and stability. Furthermore, microencapsulation via the SD
technology could store many volatile compounds with an improved
4.1. Fluidized bed coating fraction of ketones, aldehydes, alcohols, and other compounds.
It is well known and documented extensively that the SD process has
Fluidized bed coating involves encapsulating bioactive ingredients a negative impact on volatile substances due to the high temperatures
by suspending them into the air and then spraying the encapsulation employed. In this regard, an alternative approach was adopted by de
material to obtain particles. Some of the beneficial aspects of this Melo Ramos et al. (2019), wherein the vacuum SD technique was

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Fig. 1. Schematic view of the electrospinning process for preparing flavor-cyclodextrin-inclusion complex polymeric nanofibers and flavor-CD-IC poly­
mer-free nanofibers. Adapted with permission from (Saffarionpour, 2019).

evaluated to encapsulate orange essential oil. The encapsulation per­ pungency aversion.
formance of orange essential oil employing the vacuum SD (pressure
with inlet/outlet temperatures of 190 ◦ C/90 ◦ C and 10–15 kPa pressure) 4.3. Freeze-drying
was higher (99.89%) than conventional SD process. Additionally, the
vacuum SD microparticles exhibited lower mean diameter and wetta­ The freeze-drying process has been employed to generate powders
bility than those from conventional SD. Nevertheless, the technique with complex properties. Since the feed emulsion is frozen at very low
requires further exploration and development, with more experimen­ temperatures, it is ideal for encapsulating susceptible bioactive com­
tation to encapsulate other flavor compounds. pounds. The frozen solution is then exposed to extremely low temper­
Spray chilling is a technique that works in the same way as SD. The atures, which causes the ice crystals to sublimate. Since it necessitates
most significant distinction between the two methods is particle pro­ the use of a vacuum pump, it is a costly drying technology. Conse­
cessing, where the particles are created by cooling and hardening quently, the entire drying process (24–48 h) consumes a significant
droplets rather than solvent evaporation. Spray chilling may solve some amount of energy (Rezvankhah et al., 2020).
disadvantages of SD because it uses an opposite approach in which The use of freeze-drying post micro-fluidization for condensed va­
bioactive substances are spread in a liquefied matrix and atomized into a nilla extract encapsulation was performed by Ocampo-Salinas et al.
cool atmosphere like cool air. Lipids with a high melting point are often (2017), using maltodextrins with different dextrose equivalent (DE)
employed as matrices. These lipids solidify at low temperatures, thereby values as coating products. The study revealed the capacity of freeze-
immobilizing labile compounds like mineral salts, enzymes, flavors, and drying to produce matrix-type microcapsules of vanilla extract with
vitamins (de Souza Simões et al., 2017). Interestingly, a study by Günel high encapsulation efficiency (>95%). Freeze-drying was employed for
et al. (2021) that employed spray chilling could successfully suppress successfully encapsulating limonin using β-CD with a core to coating
capsaicin’s pungency, although its biological activity has been pre­ ratio of 1:10 and 1:20 and showed an efficiency of 68.14% for 1:10 and
served. As opposed to pure capsaicin, the Scoville Heat Unit (SHU) of the 80.52% for the ratio 1:20.
encapsulated capsaicin powder was reduced by 4500 times. This study
promoted spray chilling microencapsulation of capsaicin at the com­
mercial stage to make it edible for those who cannot consume it due to

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Table 1
Recent advances in the micro- and nanoencapsulation of flavoring agents.
Techniques of Flavoring agent Micro/ Encapsulants Process Specifications Major Findings References
Encapsulation Nano

Bioactive Limonene from Nano High amylose corn starch HACS + limonene • Limonene-loaded amylose (Ganje et al., 2019)
nanocarrier orange peel oil (HACS) suspension sonicated for nanocarriers loaded had
9 or 18 min (power 100 high stability against acidic
w, frequency 30 kHz). conditions with < 5%
limonene release from
nanocarriers at 37 ◦ C/2 h.
• Highest EE 85% with
loading efficiency 1.63%
• High accuracy of fuzzy
models confirmed by 0.99
minimum coefficient of
determination between the
predicted and experimental
values.
Coaxial Aqueous saffron Nano Zein, Tragacanth Voltage: 11, 15, 19 and • Nanofibers diameter: (Dehcheshmeh and
electrospinning extract 23 kV; 95–271 nm. Fathi, 2019)
Nozzle-collector distance: • LC: 3.57–9.52%
14.5 cm • EE: 60.89–91.55%,
Flow rate: 0.19 mL/h. • Release of saffron extract at
21.66, 27.75, 43.88, and
16.12% in saliva, hot water,
gastric and intestinal media,
respectively.
Complex β-pinene Micro Sodium caseinate, Formulations varied by: • The retention time-course of (Koupantsis and
coacervation Carboxymethylcellulose Protein: polysaccharide; β-pinene fitted well to Avra­ Paraskevopoulou, 2017)
β-pinene: wall materials; mi’s equation.
reticulating agents: • Glycerol addition resulted in
glycerol or tannic acid. higher retention of the
volatile compound in the
powder stored at low RH
and temperature (0% RH,
25 ◦ C)
Complex Black pepper Micro β-lactoglobulin, sodium • Optimal ratio of 17:1 (Bastos et al., 2020)
coacervation essential oil (Piper alginate, transglutaminase (β-lactoglobulin: sodium
nigrum L.) (cross-linking) alginate) at a pH of 4.5 for
complex formation with EE
of 85.01%.
• Black pepper essential oil
after digestion presented
high stability (84.8%), and
bioaccessibility (31.16%).
Complex Cinnamaldehyde Micro Gelatin, High methyl pectin Emulsification: 9000 rpm • High yield of coacervates (Muhoza et al., 2019)
coacervation (HMP), low methyl pectin for 3 min (O/W). with good size and
(LMP) pH: 4.23 (G/HMP) and morphology occurred at pH
4.37 (G/LMP). 4.23 and 4.37 for G/HMP
with a ratio of 3:1 and G/
LMP with a ratio of 6:1
respectively.
• Complex coacervation using
gelatin and pectin
significantly increased the
degradation temperature
from 180 to 220 ◦ C to
350–400 ◦ C.
Complex Oregano essential oil Nano Gelatin-Chia mucilage; Homogenization: • Characteristics peaks of (Hernández-Nava et al.,
coacervation, (OEO) (Origanum Gelatin-gum Arabic. ultrasound at 20 kHz for carvacrol, one of the 2020)
spray drying vulgare) Emulsifier: Tween 80. 10 min. majority components
pH: 3.6 present in OEO.
Spray drying: inlet • the amount of emulsifier
temperatures (180 and (Tween 80) and essential oil
160 ◦ C) and feeding rates added influenced the
(5 and 7.5 g/min) formation of coacervates,
especially the particle size.
Complex Black pepper (Piper Micro Gelatin, sodium alginate, Homogenization: 10,000 • β-caryophyllene from black (Heckert Bastos et al.,
coacervation, nigrum L.) essential calcium chloride; rpm, 30 min at 25 ◦ C. pepper EO was major 2020)
freeze-drying oil Emulsifier: Tween 20. pH adjustment: 4.0 terpene identified.
• The ratio of 6:1 (gelatin/
sodium alginate) at pH 4.0
was the ideal condition.
• The encapsulation efficiency
varied from 49.13 to
82.36%,

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Table 1 (continued )
Techniques of Flavoring agent Micro/ Encapsulants Process Specifications Major Findings References
Encapsulation Nano

Complex Ginger essential oil Whey Protein isolate/gum Optimum pH: WPI/GA • Best complex coacervate (Tavares and Noreña,
coacervation, (Zingiberisrhizoma Arabic (WPI/GA); gum (3.75) and GA/C (3.6) yields (43 and 73%) were 2020)
freeze-drying L.) Arabic/chitosan (GA/C). freeze-drying: − 57 ◦ C/ obtained when using mass
pressure < 130 μmHg. ratios of 3:1 (w:w), for WPI/
GA, and of 5:1 (w/w) for
GA/CH, respectively.
• Only physical interactions
occurred between the
functional groups of ginger
essential oil and of WPI/GA
and GA/CH complexes
Complex Michelia Alba D.C. Micro Gelatin, gum Arabic (GA) Gelatin-GA complex • Optimized formulation of (Samakradhamrongthai
coacervation, flavor powder coacervation system (pH gelatin (3.00% w/v), GA et al., 2019)
spray drying (MADFP); 4, temperature 0 ◦ C) (3.73% w/v), and
Pandanflavor Spray drying inlet and pandanflavor (5.26% w/v)
infusion. outlet temperature: exhibited high yield
150 ◦ C and 50 ◦ C. recovery with low moisture
content and low water
activity.
• Multicore capsules showed
excellent EE of MADFP
Complex Vanilla oleoresin Micro Chitosan, gum Arabic Spray drying: (100 ◦ C/ • The optimal conditions for (Hernández-Fernández
coacervation, (V. planifolia 60 ◦ C inlet/outlet the complex coacervation et al., 2020)
spray drying Andrews) temperature) process were 0.34%
Chitosan: 0.25–1.0% (w/ chitosan, 1.7% gum Arabic,
v), 5.29 pH, and an oleoresin:
Gum Arabic: 1–5% (w/v) wall material ratio of 1:2.5.
pH: 2–8. • The retention and
encapsulation efficiencies
were 84.89 ± 1.94% and
69.20 ± 1.79%.
Electrospinning Tea tree essential oil Nano Polyacrylonitrile; Voltage: 15 kV. • ElectrospunPAMAM mats (Mounesan et al., 2021)
(TEO); Eucalyptus Poly-amidoamine dendritic Distance: 10 cm. Flow displayed extended releases
essential oil (EEO) compounds (PAMAM). rate: 0.8 mL/h. for TEO (6–23 days) and
EEO (5–27 days).
• Samples contacting
PAMAMpossessed more
durable antibacterial
property.
Electrospraying Mentha longifolia L. Nano Balangu seed gum (BSG), BSG: 0.25, 0.5% w/w. • Increasing the concentration (Rezaeinia et al., 2019)
polyvinyl alcohol (PVA) PVA: 0.5, 1, 2%. of PVA enhanced LC
Tween-20 Tween 20: 0.06, 0.08, (77.56–84.68%) and EE
0.1%. (81.54–87.82%) of essential
Electrospraying: 1 mL/h oil.
pump flow rate; 25 kV • Mentha longifolia L.
voltage; needle tip-to- essential oil was entrapped
collector distance 150 in nanostructures without
mm. any chemical interaction
with encapsulant material
Emulsion Vanilla and Nano Galactan exopolysaccharide EPS: flavor (3:2) • Smooth, spherical (Kavitake et al., 2020)
cardamom flavors (EPS) Flavor emulsions: appearance with evenly
lyophilisationfreeze- dispersed particles.
dried (48 h) • Particle size: 202.34 nm for
encapsulated vanilla and
202.95 nm for encapsulated
cardamomflavors.
Emulsion Cinnamaldehyde Micro Chitosan, Pectin Chitosan (0.5%, w/v); • Ultrasonicated (Gong et al., 2020)
(ultrasonication- Pectin (0.5%, w/v); microcapsules showed
assisted), spray Chitosan, pectin: oil, higher flavor retention at
drying cinnamaldehyde (5:1 v/ high temperatures
v) (>150 ◦ C).
• Ultrasonication promoted
amide bonding of chitosan
and pectin leading to stable
capsules.
Emulsion Peppermint flavor Nano Gum Arabic Inlet, outlet temperature: • Ultrasound application for (Sangolkar et al., 2019)
(ultrasound- 170 ◦ C, 80 ◦ C. encapsulation enhanced EE
assisted); spray Flowrate: 5 mL/min to 87%.
drying Evaporation rate: 1.5 kg/ • Particle size after spray
h drying: 45.2–255.7 nm.
• Peppermint flavor
properties unaffected by
acoustic cavitation
Emulsion D-Limonene Nano Alyssum homolocarpum AHSG concentration: • Smooth and compact (Khoshakhlagh et al.,
electrospraying seed gum (AHSG) 0.25, 0.5, 0.75 or 1% (w/ capsules obtained from 2018)
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Table 1 (continued )
Techniques of Flavoring agent Micro/ Encapsulants Process Specifications Major Findings References
Encapsulation Nano

w) electrospraying of high-
Tween 20: 0.1 or 0.5% speed homogenized emul­
(w/w); sion containing 0.5% gum
D-limonene: 20% (w/w) (w/w), 20% D-limonene (w/
Homogenization: w), and 0.1% surfactant (w/
ultrasound or high-speed w) under the applied voltage
homogenizer. of 20 kV and flow rate of 0.1
mL/h.
• Average diameter: 65.68 ±
8.80 nm; EE:73.4%.
Modified CD-IC; Thymol Nano Hydroxypropyl- • Modified CD-IC were free- (Celebioglu et al.,
electrospinning β-cyclodextrin (HPβCD), standing and morphologi­ 2018b)
hydroxypropyl- cally homogenous nano­
γ-cyclodextrin (HPγCD) and fibrous webs of thymol.
methyl-β-cyclodextrin • Thymol/CD-IC nanofibers
(MβCD) exhibited antioxidant
activity with improved
water solubility and high
thermal stability of thymol.
Nanoemulsions D-limonene from Nano Oily phase: FCEO. Varying nanoemulsion • Droplet size of (Li et al., 2019)
finger citron formulations with nanoemulsions increased
essential oil (FCEO) surfactants (Cremophor from 10 to 18 nm to
EL, Tween 80®) and co- 105–1106 nm post
surfactants digestion, suggesting
coalescence or aggregation.
• Zero-order and Ritger-
Peppas model best fit models
at mouth and intestinal
stage.
β-CD-IC Vanillin Micro Flaxseed gum, Rice bran Core: Vanillin/β-CD-IC • With core: wall (1:3) and (Hasanvand and Rafe,
coacervates protein, β-CD Wall: Rice bran protein, protein: polysaccharides 2019)
Flaxseed gum, (Protein: (9:1), vanillin/β-CD-loaded
Polysaccharide ratio). microcapsules had
Core: wall (1:1, 1:2, 1:3) maximum EE of 85%.
• Increased thermostability
and shelflife of vanillin.
γ-CD-IC; freeze- Watermelon flavor Nano γ-CD γ-CD: watermelon flavor • Average particle size: 111.5 (Xiao et al., 2019)
drying mass ratio equal to 3:1 ± 6 nm; PDI: 0.237.
Pre-freeze: − 20 ◦ C/24 h • Watermelon-flavored CD-IC
Vacuum freeze-drying: had clear, uniform, and
− 50 ◦ C/24 h. unimodal particle size
distribution.
• Thermal evaporation of
watermelon flavor shifted to
higher temperatures due to
interaction in complexation.
Spray and freeze- Strawberry Micro maltodextrin, soluble fiber, Optimum conditions • Spray-dried: spherical, (Balci-Torun and
drying modified starch, were; air inlet smooth and homogeneous. Ozdemir, 2021)
β-cyclodextrin, and Arabic temperature: 190 ◦ C, • Freeze-dried: heterogeneous
gum maltodextrin: 15.30%, and spongy.
modified starch:1.83% • Particle size of the spray-
and Arabic gam: 12.87%. dried(D90 value:22.91 μm)
much lower than freeze-
dried (D90 value:326.83
μm)
Spray-chilling 2-Acetyl-1-pyrroline Micro Paraffin • Greater 2AP stability (Yin and Cadwallader,
(2AP) • Application in instant rice 2019)
• Full flavor recovery with
controlled release
Lactose-Whey Ethyl acetate Micro Lactose, WPI Lactose: WPI (0:1, 1:1, • EA particles accumulated (Huang et al., 2021)
protein isolate 1:4, 4:1) and migrated to powder
(WPI) Emulsion freezing: surface resulting in EA
microcarriers, − 24 ◦ C for 24 h and flavor release.
emulsion, freeze- − 80 ◦ C for 6 h. • Lactose crystallization
drying Freeze-drying: − 40 ◦ C for caused structural
48 h, <0.1 mbar. modification of
microparticles.

PDI: Polydispersity index; EE: Encapsulation efficiency, CD-IC: Cyclodextrin inclusion complex; LC: Loading capacity.

4.4. Electrospinning/electrospraying or nanoscale fibers and capsules, respectively (Castro Coelho et al.,
2021). An electrospraying/spinning set-up includes a high voltage
Electrohydrodynamic techniques employed for encapsulation source, a syringe pump, a blunt-end stainless steel needle, and a
include electrospinning and electrospraying that use high voltage elec­ grounded collector, as observed in the schematic diagram depicting the
trostatic fields on polymer solutions to produce continuous sub-micron electrospinning process in Fig. 1 (Frakolaki et al., 2020). The jet exits as

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a fiber at a high polymer solution concentration (electrospinning), gelatin and GA system. The Gelatin-chia system had a higher encapsu­
leading to solid nanofibers deposition. At lower concentrations (elec­ lation efficiency at 160 ◦ C than gelatin-GA at 180 ◦ C. This variation was
trospraying), droplet formation occurs wherein, upon solvent evapora­ explained by the lower mass transfer rate required for the gelatin-chia to
tion, solidifies to deposit nanoparticles and nanoclusters on the collector permit the water bound to the mucilage gel to evaporate and form
(do Evangelho et al., 2019). Coaxial electrospinning/spraying comprises capsules with a smooth surface. Contrarily, there is an increased need for
an outer and inner capillary tube or needle, each fed with two different the mass transfer rate permitting rapid encapsulant drying in the gelatin-
polymer solutions (Gómez-Mascaraque et al., 2019). GA system. Nevertheless, the feeding rate would have permitted enough
Electrospinning/spraying technique generates nano/microstructures moisture into the capsule to prevent surface cracks in the gelatin-GA
with increased surface-area-to-volume ratio, high inter-intra pores, and system.
encapsulation efficiency, improved physical and functional character­ The complex coacervation process for protein and polysaccharide-
istics, and enhanced protection of compounds of interest (Castro Coelho based encapsulants occurs over a narrow pH range between the pKa of
et al., 2021; Dehcheshmeh and Fathi, 2019; Gómez-Mascaraque et al., reactive groups along the anionic polysaccharide backbone and iso­
2019). Aside from being cost effective, it does not involve heating, and electric point (pI) of the protein (Heckert Bastos et al., 2020). Micro­
maintains the bioactive components’ properties (Castro Coelho et al., capsule formation occurs due to protonated amino groups (protein) and
2021). The advancements in electrospinning are numerous in terms of the de-protonated carboxyl group (polysaccharide) interactions. In this
controlled and sustained release, tunable porosity, mechanical endur­ regard, Heckert Bastos et al. (2020) emphasized the protein-
ance, biocompatibility, and high loading capacity (Balusamy et al., polysaccharide interaction of encapsulants to protect black pepper
2020). essential oil and its terpenes. The study employed sodium alginate and
The research conducted by Rezaeinia et al. (2019) studied the elec­ gelatin as encapsulants for complex coacervation. Gelatin has a pI of 5.0,
trospraying of Lallemantia royleana (Balangu) seed gum for Mentha and sodium alginate has a pKa between pH 3.4–3.7. At pH < pKa, the
longifolia L. essential oil release. The best-suited jet mode for electro­ turbidity noticed results from the protonation of sodium alginate’s
spraying was the cone-jet mode, since it had higher stability and spray carboxylic group (–COO– → –COOH+) besides aggregation. The pH
ability. This mode was noticed when the essential oil emulsion formu­ 4.0 was favorable for complex coacervate formation between gelatin
lations comprising 1% polyvinyl alcohol (PVA), 0.25% Balangu seed and sodium alginate at 6:1 ratio, which was indicated by increased
gum, and 0.08% Tween-20 were electrosprayed. An increase in PVA turbidity (65.2 ± 0.24).
concentration from 0.5 to 1% improved encapsulation efficiency and
loading capacity of flavor nanocapsules from 81.54 to 87.82% and 77.56 4.6. Emulsification
to 84.68%, respectively. It could be stipulated that increased emulsion
viscosity improved the stability, loading capacity, and encapsulation Emulsification is employed as a preparatory step for other encapsu­
efficiency. lation techniques, such as SD, electrospraying, and freeze-drying (Sai­
Another recent study by Wu et al. (2020) employed PVA for fullah et al., 2019). Emulsions usually involve two immiscible liquids,
obtaining electrospun nanofibrous films composed of menthol/β-CD-ICs where one is dispersed as spherical droplets within the other (Cox et al.,
for smoke filtration and flavor retention. After storage for 22 days, the 2020). An oil-in-water (O/W) emulsion is the dispersion of oil droplets
menthol retention in PVA films was 74%. Furthermore, the stable in­ in an aqueous continuous phase, whereas a water-in-oil (W/O) emulsion
clusion of menthol in host molecule β-CD ensured a sustained release occurs when the continuous phase is fat, and the dispersion phase is
profile from the nanofiber films, vital for volatile flavor retention. water. For O/W emulsions, flavor components are transferred from oil
Doping menthol/β-CDICs into the PVA nanofiber films by electro­ droplets to the aqueous phase before release from the aqueous phase
spinning could further decrease the menthol release rate. into an air (vapor) phase (Tamaru et al., 2018). Other complex emul­
Other instances of electrospinning/spraying for flavor encapsulation sions include oil-in-water-in-oil (O/W/O) and water-in-oil-in-water (W/
have been mentioned in Table 1. O/W) double emulsions that comprise other emulsions inside the
droplets given their compartmentalized structure (Yang et al., 2021).
4.5. Coacervation While conventional emulsions require only one emulsifier, double
emulsions need a lipophilic emulsifier for water droplets and a hydro­
Mixing two opposite polyelectrolytes results in an electrostatic philic emulsifier for oil droplets (Leister and Karbstein, 2020).
complex formation that may be insoluble or soluble. Based on the type Pickering stabilization is based on the interfacial adsorption of bio­
and characteristics of polyelectrolytes, insoluble complexes form ag­ logical particles rather than synthetic surfactants. They are highly
gregates or coacervates (Muhoza et al., 2020). Coacervation, or liquid­ resilient to coalescence during storage and post oral administration and
–liquid phase separation, is a spontaneous process wherein a have high interfacial area and increased stability against coalescence
homogenous colloidal solution separates into two immiscible liquid (Troise et al., 2020; Guan et al., 2021). To increase the free fatty acids
phases in one solvent. Coacervate is the dense phase containing higher flavor release for low-fat cheeses during lipase hydrolysis, Guan et al.
amounts of colloids, whereas the one with lesser colloids in equilibrium (2021) immobilized lipases on α-lactalbumin nanotubes (lipase-nano­
with the dilute liquid phase is the equilibrium phase (Zhou et al., 2020). tubes) for stabilizing O/W Pickering emulsions. The study found that
Coacervation is induced by altering the pH, temperature, ionic strength, lipase-nanotube emulsions improved the lipase catalytic efficiency and
solubility, stirring rate, biopolymer ratio, molecular weight, and hydrolyzed the release of 1.5 times higher quantities of free fatty acids
biopolymer concentration (Timilsena et al., 2019; Muhoza et al., 2020). flavor than free lipases with similar triglycerides. The Pickering emul­
Simple coacervation consists of a single biopolymer whereas, com­ sions significantly enhanced the interfacial area between lipases and the
plex coacervation comprises two or more biopolymers (Samakradham­ oil phase, leading to a higher hydrolysis efficiency.
rongthai et al., 2019). Complex coacervation deals with associative To enhance the heat stability of cinnamon flavor during baking,
interactions between oppositely charged polymers (protein and poly­ Gong et al. (2020) employed an ultrasonication-assisted microencap­
saccharide), promoted by H-bonding, hydrophobic, and electrostatic sulation technique with chitosan and pectin using the induced cross­
interactions (Lemos et al., 2017). Various advantages include high linking approach. Ultrasonication employs high-intensity sonic waves of
encapsulation efficiency, low encapsulant concentration, appreciable frequencies at 20 kHz or more to produce agitation. The agitation gen­
encapsulant integrity, and employing a wide range of biopolymers as erates cavities of gas or liquid within the system with the capacity of
encapsulants (Heckert Bastos et al., 2020). Hernández-Nava et al. (2020) implosion. The energy released from cavitation induces water to
investigated the encapsulation of oregano essential oil focussing on generate free radicals that further aid in the chemical bonding of
gelatin-chia mucilage encapsulation system and compared it with the encapsulants for microcapsule formation. The study found that with

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Table 2
Application of flavor encapsulation systems in food.
Techniques of Flavor agent Specifications of encapsulation Food-based Salient Findings References
Encapsulation system applications

Pickering emulsions Lipases α-lactalbumin nanotubes Low-fat cheeses • Promotion of free fatty acidflavor release observed upon (Guan et al.,
lipase-nanotubes emulsion addition in low-fat cheeses. 2021)
• Lipase-nanotubes emulsion addition resulted in enlarged
interfacial area.
Emulsions, freeze- Cardamom and Galactan exopolysaccharide (EPS)- Muffins • Galactan (EPS)-based vanilla incorporation reduced (Kavitake
drying vanilla based emulsion-lyophilization. hardness, increased springiness, and cohesiveness of et al., 2020)
muffins.
• Enhanced acceptability and positive valorization of the
galactan-EPS based vanilla muffin
Electrospinning Cinnamic Needle-less electrospun zein Sausages • Improved antioxidant activity observed in electrospun (Karim et al.,
aldehyde nanofibers of cinnamic aldehyde zein nanofibers containing cinnamic aldehyde during 2021)
storage.
• Enhanced anti-bactericidal effects against E. coli O157:H7
and S. aureusPTCC 1337 observed in electrospun, encap­
sulated cinnamic aldehyde.
• No adverse effects on color, texture profile, and sensory
properties of sausages.

cavitation and free radical presence, aqueous chitosan and pectin could 2020). They possess a hollow structure and are shaped like a truncated
suitably form linkages and encapsulate the hydrophobic cinnamalde­ cone. CDs are composed of glucose units covalently bound and linked by
hyde. The study also established that, since chitosan and pectin possess oxygen and held together by H-bonding between hydroxyl groups at the
good emulsifying properties, there was increased flavor retention in a cavity with a wider rim (Saffarionpour, 2019). CDs characteristically
stable cinnamaldehyde emulsion. Other instances of the applications of possess a hydrophobic internal cavity for complex formation with guest
flavor encapsulation in food systems have been summarized in Table 2. molecules for encapsulation structure formation (Carneiro et al., 2019).
This is also suitable for inclusion complexation with several non-polar
moieties without covalent bonding (Saffarionpour, 2019). Addition­
4.7. Cyclodextrins inclusion complexation
ally, aggregates with smaller molecules influence their solubility and
interactions with other molecules in complex matrices (Radić et al.,
Cyclodextrins (CDs) are cyclic oligosaccharides (α-CD, β-CD, and
2020). CD-based encapsulation enhances the stability of bioactive
γ-CD), composed of six, seven, or eight glucosyl units (Perinelli et al.,

Fig. 2. Depiction of encapsulation employing CPF technology with LCY, hydrated as limonene content of the emulsion-loaded yeast cells and LCY, dried the
limonene content of the dried limonene-filled yeast cells. Adapted with permission from (Errenst et al., 2021).

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agents in the gastrointestinal tract by decreasing the rate of hydrolysis, soluble, and gelatinized polymer under wet conditions. This phenome­
oxidation, racemization, stearic rearrangement, enzymatic decomposi­ non was observed with the rapid release of both flavors within 10 min
tion, or complex formation with other food components that signifi­ upon water addition at 105 ◦ C. This study correlated the flavor release
cantly affects bio-accessibility (Carneiro et al., 2019; Saffarionpour, behavior using Gaussian distribution of activation energy of the first-
2019). The complex formation of CDs is exploited for flavor encapsu­ order release rate constant. The activation energy ranged at 50–55 kJ/
lation and preservation (Saffarionpour, 2019). mol and 76–116 kJ/mol for both flavors under wet and dry conditions,
Celebioglu et al. (2018a) employed modified cyclodextrins inclusion respectively.
complexes (CD-IC) Hydroxypropyl-β-CD-IC (HPβCD-IC), HPγCD-IC for
electrospinning cineole, and p-cymene to produce nanofibrous webs 5. Controlled release of flavor compounds
without employing polymeric carrier matrices. A general trend observed
when solutions with high conductivity and low viscosity are electrospun Controlled release and stability are essential features of encapsula­
is the formation of thinner fibers, because of increased stretching of the tion systems. Controlled release ensures that compounds of interest are
jet. A similar outcome was observed in this study for CD-IC-nanofibers liberated at a specific rate over a prolonged duration, reducing core
where p-cymene/HPβCD-IC (550 nm) had the lowest average diameter, compound loss during processing operations (Sultana et al., 2018).
and the cineole/HPγCD-IC (785 nm) possessed the highest average Evaluating the controlled release of encapsulated flavors is ideal for
diameter. A key difference between the two nanofibers was that p- predicting the flavor availability throughout the process or storage
cymene/HPβCD-IC had lower viscosity (~0.30 Pa.s), enabling greater period (de Souza et al., 2018). The flavor release rate is defined as flavor
stretching and resulting in thinner fibers production during molecules migrating from one environment/state to another over a
electrospinning. certain time. Monitoring the flavor and aroma compounds’ release rate
Although CDs are considered GRAS, its type and mode of adminis­ is highly essential for food products. Consumers can perceive the taste
tration significantly influenced its safety and toxicity. They are practi­ and quality of food products even before direct consumption. This is
cally non-toxic, because of their bulky and hydrophilic nature. When because the volatile flavors combined with the air molecules enter the
administered orally, there is negligible absorption in the gastrointestinal nasal cavity, contact the olfactory epithelium receptor cells via the ortho-
tract. Nevertheless, high doses of CDs might be harmful and cause nasal route, and the human brain perceives the quality and taste of food
irreversible kidney damage and dysfunction (Carneiro et al., 2019). (Saifullah et al., 2019).

4.8. Yeast cell microcarriers 5.1. Role of encapsulants in flavor compounds release from encapsulation
systems
Implementing cell-based micro-carriers for encapsulation is
increasingly prevalent for several food-grade substances in the past few Since the effectiveness of encapsulation structures rely on the sta­
decades. Of these, yeast cells (Saccharomyces cerevisiae) are predominant bility of encapsulants chosen, the choice of coating materials employed
as a low-cost encapsulant, with their cell envelope playing the role of determine the overall success of the process. The primary role of
coating material (Karaman, 2020). Yeast has a simplified structure encapsulants is to protect the core compound by acting as a barrier
considering its lack of complexity, no additive requirements, and against external factors and preventing reactions with other compo­
cell–cell binding (Young et al., 2020; Karaman, 2020; Sultana et al., nents. Encapsulants should also possess properties suitable for the cho­
2018). They possess a phospholipid membrane that acts like a liposome sen method of encapsulation; for instance, attaining a high stability and
for successfully encapsulating both hydrophobic and hydrophilic mol­ flavor release at specific durations and desired locations (Balci-Torun
ecules (Fu et al., 2021). The cell wall of yeasts provides good mechanical and Ozdemir, 2021). Encapsulants comprise of hydrophilic and hydro­
strength and permits molecules up to 400 kDa to move freely. In this phobic polymers that form polymeric networks to hold the core com­
regard, flavor compounds can pass through the lipid bilayer membrane pound within the matrix. A combination of polymers is chosen, since it
with ease, as the molecular weight of flavoring agents is lower than 400 guarantees improved barrier properties compared to a single polymer
kDa (Sultana et al., 2018). Furthermore, yeasts are easier to the culture (de Souza et al., 2018).
at an industrial scale (Young and Nitin, 2019). In flavor and aroma encapsulation, the encapsulant primarily in­
Using condensed powder type (CPF) technology, Errenst et al. (2021) fluences the total aroma recovery. While encapsulating strawberry fla­
successfully encapsulated limonene flavor into yeast cells. This high- vor, Balci-Torun and Ozdemir (2021) found that the total aroma
pressure spray process is appropriate for loading flavors under particu­ recovery was high at constant inlet temperature when maltodextrin was
larly mild conditions, like an inert gas atmosphere and low tempera­ mixed with GA, modified starch, and soluble fiber. However, when
tures. Fig. 2 depicts the yeast cell encapsulation schematically. A thin modified starch was increased, and GA or soluble fiber was decreased,
film is formed on the surface of the agglomerated yeast cells by the fine the total aroma recovery also increased. In this study, maltodextrin,
spray produced in the CPF process. This facilitates the contact between modified starch, soluble fiber, GA, and β-CD were optimized to produce
the emulsion and the yeast cell wall. Water hydration leads to cell wall minimum aroma release from strawberry-based microcapsules. The re­
swelling, further permitting the permeation of limonene into the inte­ searchers also maximized the drying efficiency, solubility, and recovery
rior. This water is removed by the drying processes, which ensures the of the aroma post-dissolution of microcapsules in water. Rezaeinia et al.
closure of the cell wall’s biopolymer network, resulting in the successful (2019) electrosprayed Lallemantia royleana (Balangu) seed gum for
encapsulation of the flavors within yeasts. The study established Mentha longifolia L. essential oil release. A faster release of the essential
encapsulation efficiencies of ~85.9% for the CPF spraying process. oil was observed in distilled water media. This was attributable to the
Similarly, in another study by Sultana et al. (2018), the release increased water solubility property of Balangu gum and PVA, resulting
behavior of the flavoring compounds D-limonene (hydrophobic) and in higher solubility and swelling degree of nanocapsules.
ethyl hexanoate (hydrophilic) was studied after yeast cell encapsulation. Zarandona et al. (2020) developed CD-ICs to monitor the release of
Comparisons were made between the oxidative stability of D-limonene 2-phenyl ethanol from chitosan films. β-CD was chosen to develop CD-
in yeast and maltodextrin encapsulation systems. Interestingly, both ICs as it exhibited a greater retention yield (45%) than γ-CD (40%)
flavors were retained at ~85% under dry heating at 140 ◦ C after 1 h and α-CD (32%). The relatively lower retention values could be because
incubation. This higher retention capacity of yeast cells could be of a single hydroxyl group on 2-phenyl ethanol for its attachment to CDs
attributed to β-glucans, a water-soluble carbohydrate fiber on the yeast and, weakening the interaction. The results showed that 2-phenyl
surface, which acts as a wall material. Another interesting property of ethanol evaporated with only 8% retention in the films without ICs,
β-glucans is its ability to transform from a hard, glassy state to a soft, whereas >90% retention was seen in films with ICs. Furthermore, the

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that moisture sorption of the yeast cells led to the swelling of the cell
wall’s protein layer, which then generated holes and perforations. This
mechanism facilitated the release of volatile flavor compounds from the
cells. Nevertheless, the moisture absorption of the external layer resul­
ted in its uncontrolled swelling, causing the breakdown of cell protec­
tion and permitting the exchange of flavor with the outside media.

5.3. Controlled-release kinetic models

5.3.1. Burst release


The various release models for the controlled release from encap­
sulation systems can be found in Fig. 3. The rapid release of the core
compounds from encapsulation systems in a short duration comprises
burst release (Boostani and Jafari, 2021). In a mathematical and fuzzy
Fig. 3. Different release profiles for encapsulated systems. Adapted with model release study conducted on amylose nanostructures containing
permission from (Boostani and Jafari, 2021). limonene, Ganje et al. (2019) observed that by increasing the amylose
nanocarrier’s size from 5.65 to 41.9 nm, the quantity of limonene
fast flavor release occurred 4 h after immersion in 95% ethanol, released in the intestinal environment declined from 79 to 40%, which is
attributable to the weak interactions with β-CD. Huang et al. (2021) approximately a 50% decrease. Reducing the nanocarriers size resulted
studied the release of ethyl acetate from lactose-whey protein isolate in a higher surface-area-to-volume ratio, increased enzyme availability
matrices, which was based on the lactose crystallization and micro­ for amylose helix deconstruction, thereby increasing the limonene
structure of the particles. They observed that microparticles with high release rate. Decreasing the amylose levels resulted in an increased in­
lactose exhibited the lowest flavor retention, whereas rapid flavor testinal enzyme sensitivity and the release took place with a greater
release was seen at high relative humidity conditions. This could be slope with higher ingestion. The mechanical stress increased the limo­
explained by the crystallization stage of lactose, during which the nene release rate in all samples by augmenting the sonication time. This
lactose molecules released water molecules and were converted to is because increasing the process duration aggravated the particle wall
α-lactose monohydrates. This was observed by the increase in size and deterioration, which made the enzymes increasingly accessible. In this
and structural modifications of lactose particles from needle-shapes to study, the burst release index, defined for the initial time of entry into
rectangular structures. This phenomenon may have increased their the small intestine, exhibited an ascending trend with increased nano­
volume and brought about the disruption of encapsulation structures. carriers size. The limonene trapped between the amylose helices was
Due to powder surface and internal matrix restructuring, the flavors responsible for the initial burst release. This was because larger nano­
accumulated into large agglomerated particles and were prone to particles have more limonene molecules between the amylose helices
migration from the core to the surface. Therefore, the study established than smaller particles. Therefore, a higher initial burst release was
that the lactose content, surrounding humidity, and storage time observed for the former.
significantly affected the flavor retention and crystallization behavior.
5.3.2. Sustained release
5.2. Mechanisms of release of flavor compounds In a study by Xiao et al. (2019), the inclusion and sustained release
behavior of watermelon flavor encapsulated in γ-CD was investigated.
Various studies have explored flavor release behaviors from encap­ They found that the molecular structures of the flavors significantly
sulation systems. Mechanisms of the release include diffusion, swelling, influenced both inclusion and release behavior. The descending order of
melting, and degradation (Sultana et al., 2018). Flavors diffusing flavor inclusion efficiency was alcohols > aldehydes > esters. The
through particle-matrices into the external/surrounding medium caused release ratio declined with an increase in the hydrophobicity of flavor
diffusion, a predominant flavor release mechanism from encapsulation compounds, attributable to the differing affinities of hydrophobic fla­
systems. The particle–matrix may be intact throughout or alter its vors to γ-CD. The study speculated that γ-CD and watermelon flavor
properties (erosion, fragmentation, or dissolution). The flavor release interactions led to flavor compounds’ protection, possessing lower
rates from encapsulation systems rely on its relative solubility in the boiling points from rapidly evaporating. The study also concluded that
particle–matrix, the surrounding liquid and its diffusion coefficient the immense potential for the sustained-release characteristics of
through the matrix (Bastos et al., 2020). watermelon flavor-CD-ICs was as expected.
Samakradhamrongthai et al. (2019) developed a multi-core encap­
sulated flavor powder using gelatin, GA, infused with Pandan flavor. The 5.3.3. Delayed release
release rate constant of Pandan was calculated by employing Avrami’s In the delayed-release design, the aim is to release separate com­
equation (Weibull distribution function). The Avrami’s parameter, ‘n,’ pounds at later times. The release of the encapsulated compounds is
ranged from 0.25 to 3.74, suggesting that the flavor release mechanism delayed from a limited lag time until the release is found suitable and
could be molecular diffusion (n < 1), the first-order mechanism (n = 1), desirable (Boostani and Jafari, 2021). Wang et al. (2019) showed that
and rapid release with an induction period (n > 1). The n values in the the encapsulation of allyl methyl disulfide-loaded lipid droplets in
study ranged from 0.14 to 0.45, implying that the diffusion mechanism biopolymer-based microgels delayed flavor release appreciably up to 3-
governed the flavor release. fold longer. Theoretically analyzing the flavor release suggested that its
Sultana and Yoshii (2019) analyzed the release profile of flavoring retention was enhanced with an increase in the microgel size or oil
compounds d-limonene and ethyl hexanoate using a complex vapor droplet concentration. The microgels diameter (270 μm) were initially
sorption method. The flavors were spray-dried and encapsulated using >1000-fold greater than the lipid droplets diameter (0.26 μm) in the
yeast cells (Saccharomyces cerevisiae), from which β-glucan was partially emulsions, causing a much slower release rate. Furthermore, the phys­
extracted. Although the study successfully encapsulated the flavor in ical interactions of the flavor molecules with the biopolymer network
yeast cells, not all flavors could penetrate the lipid bilayer membrane, results in binding, which causes slower release and leads to delayed
with some flavor retained near the yeast cell wall. The mode of flavor release mechanism.
release from the encapsulated yeast cells could either be by its evapo­
ration through holes or diffusion through the cell wall. The study found

11
Table 3

Y. Premjit et al.
Empirical and semi-empirical models for fitting the release of flavoring agents from encapsulation systems.
Kinetic model Equation Specifications Salient features References

Zero order C=Kt C = amount of released (Li et al., 2019; Ganje et al., 2019; Dehcheshmeh and Fathi, 2019; Bastos et al., 2020)
flavor at time, t;
K = Kinetic constant
First order Ln C = K t C = amount of released Release of loaded (Ganje et al., 2019; Dehcheshmeh and Fathi, 2019; Bastos et al., 2020; Rezaeinia et al., 2019)
flavor at time, t; compounds from porous
K = Kinetic constant structures.
Higuchi C = K t0.5 C = amount of released (Dehcheshmeh and Fathi, 2019; Bastos et al., 2020)
flavor at time, t;
K = Kinetic constant
Ritger-Peppas C = K tn C = amount of released • n < 0.45: release (Li et al., 2019; Bastos et al., 2020; Dehcheshmeh and Fathi, 2019)
flavor at time, t; mechanism is Fickian
K = Kinetic constant diffusion;
n = release power • n > 0.89: swelling-
controlled system;
• 0.45 < n < 0.89:
diffusion and swelling
Peppas-Sahlin C = k1 tm + k2 t2m C = amount of released • To evaluate the (Dehcheshmeh and Fathi, 2019; Rezaeinia et al., 2019)
flavor at time, t; mechanism of Fickian
k1 = diffusion rate and non-Fickian trans­
(Fickian) constant. fer from the structure
k2 = erosion rate constant of delivery systems.
m = purely Fickian • k1/k2 > 1: diffusion
diffusion exponent for a • k1/k2 < 1: erosion.
system of any • k1/k2 = 1: both
configuration. Fickian diffusion and
erosion mechanisms.
Weibull log (-ln (1- C)) = b (log(t) C = amount of released (Sultana and Yoshii, 2019)
12

– log (a)) flavor at time, t;


a, b = shape parameters
of Weibull model
Koptcha C = A(t)0.5 + B(t) C = amount of released • To evaluate the release (Dehcheshmeh and Fathi, 2019; Rezaeinia et al., 2019)
flavor at time, t; of bioactive
A, B = kinetic constants compounds from
delivery systems by
diffusion or erosion
mechanisms.
• The A/B ratio is used to
predict the dominant
mechanism of flavor
release.
• A/B > 1: diffusion.
• A/B < 1: erosion.

Food Research International 151 (2022) 110879


• A/B = 1, both diffusion
and erosion.
Avrami equation Y = 1 − exp (ktn) Y = release fraction of • n = 0.54: diffusion- (Xiao et al., 2019; Koupantsis and Paraskevopoulou, 2017)
flavor from encapsulation limited release.
system; • n = 0: Zero-order
t = release time; release kinetics (gentle
k = release rate constant; release throughout the
n = Avrami parameter release process).
(release mechanism). • n = 1: First-order
release kinetics (im­
mediate release in the
initial stage and a mild
(continued on next page)
Y. Premjit et al. Food Research International 151 (2022) 110879

5.4. Empirical and semi-empirical models of flavor release

Mathematical modelling is an appropriate method for determining


and designing formulations and further evaluating the release of com­
ponents in vitro and in vivo conditions. It aids in determining vital
physical parameters and fitting experimental data with intended models
appropriately. It is employed for theoretically predicting the factors
affecting controlled disassembly, including the type of bioactive com­
ponents and encapsulants, and the shape and size of the network (Ganje
et al., 2019).
The kinetic data on the release behavior of different flavors from
encapsulation systems are evaluated by employing theoretical, empir­
ical, or semi-empirical equations (Flores and Kong, 2017). Several
equations are reported extensively in studies, including zero-order, first-
order, Higuchi, and Korsmeyer-Peppas equations, and described in
Table 3. Flavor release kinetics follows the application of mathematical
models, such as Avrami’s equation. This equation was initially devel­
oped for the crystallization process but has been found to suitably
correlate retention with the release time in storage of various flavor
encapsulation systems (Koupantsis and Paraskevopoulou, 2017).

6. Conclusion
(Li et al., 2019)

(Li et al., 2019)

Flavors are commonly used in various food commodities and play an


References

essential part in everyday life. Flavors, made of volatile aroma com­


pounds, do not last long in the air, particularly at high temperatures.
Several studies have established that encapsulation techniques permit
the increased stability of flavoring compounds for suitable food-based
applications. The present review concluded that nanoencapsulation al­
lows for improved loading capacity, encapsulation efficiency, stability,
mechanism of release

and well-regulated flavor release profile than conventional microen­


release in the later

capsulation techniques. It is essential to point out that some microen­


prolonged stage).

• Estimation of the

from polymeric

capsulation techniques, such as spray chilling and yeast carriers, are


Salient features

gaining significant traction for their improved effect compared to the


systems

conventional techniques. Nanoencapsulation employing electrospraying


and electrospinning seems to be a more promising approach for
improving the flavor encapsulation efficiency. Another trend is the
combined application of two encapsulation techniques to attain specific
characteristics, such as emulsification or coacervation with SD, freeze-
drying, electrospraying, or electrospinning, for better effects.
Q = fractional release of

Q = fractional release of

7. Future directions
k = rate constant;

k = rate constant;
flavor in time t;

flavor in time t;
Specifications

b = constant.

b = constant.

Layer-by-layer self-assembly technology, a strategy that enables the


encapsulation of substances wherein the thickness can be controlled, is
becoming more common in developing multilayer controlled delivery
systems at the micro and nanoscale. Several novel methods of flavor
encapsulation, such as yeasts as flavor carriers, need further exploration.
Despite the potential of yeast as carriers, not much research has been
conducted to examine if these cells structures have a prophylactic effect
(100 − Q)1/3 = − kt + b

(100 − Q)1/2 = − kt + b

against thermally- or oxidatively-induced degradation of encapsulated


bioactive compounds. Further studies could emphasize various flavor
release mechanisms and the suitability and efficiency of application in a
wide variety of food systems or simulated food models. It is evident that
the breakdown dynamics of food in the mouth influences the release rate
Equation

of flavors during chewing.. Future research could be focussed on


exploring the exact mechanisms and oral phase simulations for encap­
sulated flavor release. Detailed analysis of the storage behavior of flavor
encapsulated powder is also required for integrating it with the latest
advances in commercialization.
Table 3 (continued )

Declaration of Competing Interest


Hixon-Crowell
Kinetic model

Neibergull

The authors declare that they have no known competing financial


interests or personal relationships that could have appeared to influence
the work reported in this paper.

13
Y. Premjit et al. Food Research International 151 (2022) 110879

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