Carbohydrate Polymers 312 (2023) 120789

Contents lists available at ScienceDirect

Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol

Review

Advances in chitin-based nanoparticle use in biodegradable polymers:

A review
Murat Yanat *, Karin Schroën
Laboratory of Food Process Engineering, Wageningen University and Research, Bornse Weilanden 9, 6708 WG Wageningen, the Netherlands

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

Keywords: Chitin-based nanoparticles are polysaccharide materials that can be produced from a waste stream of the seafood
Chitin nanocrystals industry: crustacean shells. These nanoparticles have received exponentially growing attention, especially in the
Chitosan nanoparticles field of medicine and agriculture owing to their renewable origin, biodegradability, facile modification, and
Biodegradable plastics
functionality adjustment. Due to their exceptional mechanical strength and high surface area, chitin-based
Nanocomposites
nanoparticles are ideal candidates for reinforcing biodegradable plastics to ultimately replace traditional plas­
Polylactic acid
tics. This review discusses the preparation methods for chitin-based nanoparticles and their applications. Special
focus is on biodegradable plastics for food packaging making use of the features that can be created by the chitin-
based nanoparticles.

1. Introduction
Plastic is an excellent material for food packaging. It allows the goods
to reach consumers safely, and is a low-cost and lightweight material
with high strength that facilitates transport. In total, 367 million tons of
plastics were produced worldwide in 2020 and 40 % of this was used for
packaging purposes, mainly for single-use and short-term applications
(Plastics Europe, 2021). Consequently, millions of tons of non-
biodegradable plastics end up in the environment. This is a current
and future hazard for living organisms and the global ecosystem, which
makes finding immediate and sustainable solutions for this of great
relevance.
Many consider biodegradable plastics a promising option for more
sustainable production of plastics (Acquavia et al., 2021; Iwata, 2015;
Mangaraj et al., 2019) as they can be derived from renewable sources,
such as agricultural waste and feedstocks. It is good to immediately
point out that when disposed of inappropriately, also biobased plastics
will cause an environmental burden, albeit that the degradation time for
such plastics is quite shorter (in the order of 10 years) compared to that
of fossil-based plastics (centuries). There are various biodegradable
options available, including polylactic acid (PLA), poly­
hydroxyalkanoates (PHAs), starch blends, and cellulose-based plastics
(Boey et al., 2021; Diyana et al., 2021; Yaradoddi et al., 2020). These
materials do not yet possess the properties needed to replace their
petroleum-based counterparts, and are only limitedly used for food
packaging; e.g., thermoformed trays and containers for fresh fruits and
vegetables, yogurt, and prepared meals (Dybka-Stępień et al., 2021;
Nilsen-Nygaard et al., 2021). To achieve widespread use, significant
improvements are needed, particularly in terms of their barrier and
mechanical properties.
In literature, a number of options have been suggested that all
revolve around the use of a combination of materials; e.g., the use of
multi-layered films (La Fuente Arias et al., 2021; Wang et al., 2022), or
the addition of (nano-)particles to create specific functionalities such as
mechanical strength, anti-microbial effects, and so on (Garcia et al.,
2018; Liao et al., 2023; Wu et al., 2023). Although multilayer films can
have significantly better properties compared to the base materials
(Boom et al., 2011), fully biodegradable multilayer packaging that is
suitable for various types of foods remains a distant prospect. Moreover,
recycling multilayer films present additional challenges, such as iden­
tifying and separating different materials in each layer and a lack of
commercially viable methods for processing them (Alias et al., 2022;
Tartakowski, 2010). Metal-based nanoparticles, such as silver, zinc
oxide, copper, and titanium dioxide, have been reported to enhance
mechanical strength, UV-blocking capability, and provide antimicrobial
and antioxidant activity (Garcia et al., 2018; Yanat et al., 2022). How­
ever, there are concerns about the potential migration of these nano­
particles into food and the environment after disposal. To mitigate these
concerns, biodegradable nanoparticles have been considered.
For the current review, we focus on biobased and biodegradable

* Corresponding author.
E-mail addresses: murat.yanat@wur.nl (M. Yanat), karin.schroen@wur.nl (K. Schroën).

https://doi.org/10.1016/j.carbpol.2023.120789
Received 24 January 2023; Received in revised form 20 February 2023; Accepted 5 March 2023
Available online 11 March 2023
0144-8617/© 2023 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
M. Yanat and K. Schroën Carbohydrate Polymers 312 (2023) 120789

that influences the physicochemical and functional properties of chitin-

based materials, and through that their applications.
The discovery of chitin dates back to 1799, when Hatchett identified
it during the decalcification of crab shells (Hatchett, 1799). Since the
1930s, academic research on chitin and chitosan has accelerated, lead­
ing to application in various fields such as medicine in which it is used in
scaffolds and bandages, as well as in food packaging within which film
and coating applications are the most relevant ones to mention (Crini,
2019). The use of chitin-based nanomaterials (micro- and nanoparticles,
nanofibers, hydrogels) has been suggested for a wide range of applica­
Fig. 1. The chemical structures of chitin and chitosan. tions; in the following sections, we first discuss the reported preparation
routes, and next present suggested application of chitin-based
chitin-based (chitin and chitosan) nanoparticles. Researchers have nanoparticles.
suggested them (Amiri et al., 2022; Broers et al., 2018; Salaberria et al.,
2014; Scaffaro et al., 2017; Singh et al., 2020; Yanat et al., 2023) for
2.1. Preparation routes
their abundant availability in nature. They can be harvested from what
is currently considered a waste, or at most a low value, product: exo­
Crab and shrimp shells are rich in chitin, comprising 20 to 30 % of
skeletons of marine crustaceans. In this review, we report on recent
their mass (Said Al Hoqani et al., 2020; Tan et al., 2020). To obtain pure
developments in the use of chitin-based nanoparticles in biodegradable
chitin, removal of other substances such as proteins, minerals, and color
polymers. We first describe the properties of chitin nanoparticles that
pigments is needed, which can be done by chemical or biological
are obtained through the main preparation routes. We then explore how
treatment (Fig. 2). The chemical industrial extraction of chitin involves
chitin-based nanoparticles can be used to improve the physical proper­
an alkaline treatment (removal of protein) followed by an acid treatment
ties of a base polymer, including its mechanical strength and barrier
to eliminate calcium carbonate (El Knidri et al., 2018; Trung et al.,
properties, and introduce other functionalities such as antimicrobial or
2020), often carried out in conjunction with a step to remove pigments.
antioxidant effects. We wrap up with the challenges associated with
Biological extraction approaches have been geared toward reducing the
chitin-based nanoparticle use in biodegradable plastics and suggest
use of harsh chemicals (Chakravarty et al., 2018; Doan et al., 2019; Tan
potential solutions from a broader packaging perspective.
et al., 2020). Although bio-extraction of chitin at the commercial level is
still at an early stage of development, it is promising. It uses microbial
2. Chitin and chitin-based nanoparticles
fermentation; e.g., protease-producing bacteria (Pseudomonas spp.) and
lactic acid-producing bacteria (Lactobacillus spp. and Streptococcus spp.)
Chitin is the second most abundant naturally occurring poly­
are employed to eliminate proteins and minerals (Kaur & Dhillon, 2015;
saccharide that is present in the exoskeleton of crustaceans and insects,
Lv et al., 2022; Yadav et al., 2019). The properties of the thus obtained
the cell walls of fungi, and even in the beaks of octopuses (Díaz-Santana-
chitin powder may vary depending on feed source, processing methods
Iturrios et al., 2022; Hamed et al., 2016). It is composed of N-acetyl-d-
and conditions. Although the chemical extraction of chitin powder offers
glucosamine units linked by 1,4-β-glycosidic bonds, and contains a small
higher purity and yield of the end product, the biological route may have
amount of deacetylated units (2-amino-2-deoxy-D-glucose) (Salaberria,
the future due to its reduced chemical use and the potential for recov­
Labidi, & Fernandes, 2015). Chitin is insoluble in water and many
ering protein from the liquid fraction generated during the process
organic solvents due to intramolecular hydrogen bonds within the
(Arbia et al., 2013; Mohan et al., 2022).
crystalline structure. Through deacetylation, thus creating chitosan, an
Chitin powder is the basis for the production of chitin-based nano­
acid-soluble heteropolymer (containing a majority of d-glucosamine
particles; more specifically chitin nanocrystals and chitosan nano­
units; Fig. 1) is created. The degree of acetylation is the main parameter
particles. Chitin nanocrystals (also termed chitin nanoparticles, chitin

Fig. 2. Chitin extraction from crustacean's shell biowaste via chemical and biological routes.

2
M. Yanat and K. Schroën
Fig. 3. Chitin nanocrystal production routes; (A) via acid hydrolysis, (B) via TEMPO-mediated oxidation.
whiskers or nano-whiskers) are rod-like, highly crystalline (60–94 %)
small particles with a high aspect ratio (~10 nm in width and 100–600
nm in length) (Colijn et al., 2021; Fan et al., 2008; Salaberria, Labidi, &
Fernandes, 2015). These materials consist of both amorphous and
crystalline domains; the crystalline domains being known for their high
mechanical modulus (Scaffaro et al., 2017).
The primary method used for converting chitin powder into nano­
crystals is acid hydrolysis, which involves the use of highly concentrated
acid and ultrasound treatment to remove β-1-4-glycosidic bonds of
amorphous chitin regions, as shown in Fig. 3A. Typically, 3 M hydro­
chloric acid (HCl) is used at temperatures 80–110 ◦ C for 1–6 h (Ben
Cheikh et al., 2021; Liu et al., 2021; Salaberria, Labidi, & Fernandes,
2015; Scaffaro et al., 2017). The reaction can be stopped by dilution
with water. Ultrasound can be applied during and after acid hydrolysis
to facilitate the separation of amorphous and crystalline chitin regions,
as well as the dispersion of chitin nanocrystals, respectively (Colijn
et al., 2022; Yanat et al., 2022). The residual acid is removed through a
series of centrifugation, filtration, and/or washing steps. The isolation of
chitin nanocrystals is completed by a freeze-drying step. It is worth
noting that the acidic conditions during the process result in slight
deacetylation (Savitri et al., 2014; Vicente et al., 2021).
TEMPO (2,2,6,6-tetramethyl-piperidinyl-1-oxyl)-mediated oxidation
is an alternative method for chitin nanocrystal production that uses
relatively mild conditions compared to acid hydrolysis (Fig. 3B).
TEMPO-mediated oxidation selectively targets the alcoholic hydroxyl
group (the 6th carbon of the chain), and is mostly used at pH 10 (Fan
et al., 2008, 2009; Tran et al., 2019; Wu et al., 2019), with chitin
dispersed in an aqueous solution of the oxidizing agents and TEMPO
under constant stirring and pH control at room temperature. NaClO is
the main oxidant and ultrasound treatment or other mechanical disin­
tegration techniques are used to increase the formation and release of
nanocrystals (Fan et al., 2009). This technique yields highly crystalline
nanocrystals (> 90 %) without leading to deacetylation, in contrast to
acid hydrolysis (Yang et al., 2020; Ye et al., 2019).
To be complete, a few studies have reported other chemical
(ammonium persulfate (APS) oxidation, ionic liquid-based gelation) and
mechanical (grinding, high-pressure homogenization, ultrasound, and/
or their combinations) methods that were developed for the preparation
of chitin nanocrystals (Kadokawa et al., 2011; Kadokawa, 2015; Oun &
Rhim, 2017a; Duan et al., 2018).
Although the chemical structures of chitin and chitosan are very
similar, the solubility under low-acidic conditions is rather different;
3
Carbohydrate Polymers 312 (2023) 120789
chitosan is very soluble, unlike chitin (Aranaz et al., 2021; El Knidri
et al., 2018), and chitosan nanoparticles are spherical, while their chitin
counterparts are more needle-like. The most commonly employed
method for preparing chitosan nanoparticles is ionic gelation (Divya &
Jisha, 2018; Grenha, 2012; Yanat & Schroën, 2021). It is based on ionic
crosslinking between the positively charged amino groups of chitosan
and a polyanion material, typically sodium tripolyphosphate (TPP) in
low-concentration acetic acid (0.5 to 2 %) (de Pinho Neves et al., 2014;
Hamidi et al., 2021; Ismik et al., 2020). After the complete dissolution of
chitosan in the acetic acid solution, the addition of TPP solution leads to
the formation of chitosan nanoparticles. The size of these spherical
nanoparticles may be adjusted through the chitosan to TPP mass ratio,
stirring speed, and reaction temperature (Algharib et al., 2022; Sree­
kumar et al., 2018). As an alternative to TPP, anionic macromolecules
can be used in a process termed polyelectrolyte complexation, for which
sodium alginate, chondroitin sulfate or hyaluronic acid have been used
(De La Fuente et al., 2008; Sarmento et al., 2006; Yeh et al., 2011). An
alternative approach involves the radical polymerization of methacrylic
acid in the presence of chitosan to yield nanoparticles (Hasaneen et al.,
2014; Motakef Kazemi & Salimi, 2019). In general, ionic gelation-based
routes are quick and mild processes that allow precise control over the
end product, and are thus preferred.
Oil-in-water micelle structures can also be used for the production of
chitosan nanoparticles via covalent crosslinking (Zhang & Wu, 2009;
Zhang, Xu, et al., 2021; Zhang, Zhao, et al., 2021), and in literature,
there are a few examples of water-in-oil systems that lead to chitosan
nanoparticles with a particle size smaller than 100 nm (Fang et al., 2009;
Tang et al., 2007). These methods are used for spontaneous nano­
encapsulation of active ingredients in chitosan nanoparticles. For both
emulsion systems, often glutaraldehyde (GA) is used as a crosslinker.
The use of harsh solvents (n-hexane and toluene) is mentioned as the
main drawback of emulsification-based chitosan nanoparticle routes.
A few studies in literature investigate spray drying or supercritical-
CO2-assisted solubilization and atomization (SCASA) to prepare chito­
san nanoparticles (Başaran et al., 2014; Hijazi et al., 2014, 2019; Ngan
et al., 2014). Of these, spray drying is most commonly used for the
production of chitosan microparticles (or microspheres) (Katsarov et al.,
2017; Mitra & Dey, 2011; Tao et al., 2013). A top-down approach can
also be applied to create chitosan nanoparticles via deacetylation of
chitin nanocrystals by single or multi-step NaOH treatment at 80-120 ◦ C
(Wijesena et al., 2015; Yanat et al., 2022).
Table 1 provides an overview of the advantages and disadvantages of
M. Yanat and K. Schroën Carbohydrate Polymers 312 (2023) 120789

Table 1
The advantages and disadvantages of the main nanoparticle preparation methods.
Material Method Advantages Disadvantages

● Simple process ● Use of harsh chemicals

Acid hydrolysis
● Enables tailoring the nanoparticle properties ● Deacetylation of nanocrystals
Chitin nanocrystals ● Mild process
TEMPO-mediated oxidation ● Yields highly crystalline particles ● Complex application
● Deacetylation does not occur
● Simple and mild process
Ionic gelation ● Poor stability of nanoparticles in acidic conditions
● Enables tailoring the nanoparticle properties
● Complex application
Ionic gelatin with radical polymerization ● Uniformity of nanoparticles
● Time-consuming process
Chitosan nanoparticles ● Use of harsh chemical
Emulsification-based methods ● Forming ultrafine nanoparticles below 100 nm
● Complex application
● Complex application
Top-down method
● Time-consuming process
Spray drying ● Simple and mild process ● Mostly micro-sized particles occur

Fig. 4. Number of publications related to chitin-based nanoparticles (chitosan nanoparticles, and chitin nanocrystals/nanoparticles) in the last two decades
(Clarivate Analytics - Web of Science, 2023). Copyright Clarivate 2022, all rights reserved.

various chitin-based nanoparticle preparation methods. While simple
and mild processes are generally preferred, no specific method is best for
all applications.
3. Chitin-based nanoparticles in biodegradable polymers
Chitin-based nanoparticles have been getting substantial and
growing attention; Fig. 4 shows the number of published papers in the
last two decades. Clarivate Web of Science records a total of 34,910
entries (including articles and book chapters) related to chitin-based
nanoparticles, of which 32,554 pertain to chitosan nanoparticles. In
comparison, related to chitin nanocrystals (or chitin nanoparticles) 2356
entries have been indexed, indicating their relative popularity. In the
next section, we will describe the main applications of chitosan nano­
particles and chitin nanocrystals; with a particular emphasis on the use
of chitin nanocrystals in biodegradable polymers.
Chitosan nanoparticles were first described in the 1990s for the de­
livery of active compounds loaded into these particles (Alonso et al.,
1997; Ohya et al., 1994). Since then, researchers especially from the
fields of medicine and pharma have extensively researched preparation
methods and routes, and tuned particle properties through surface
modification leading to applications for cancer treatment, imaging, in­
sulin delivery, gene therapy, and many more. Moreover, multifunctional
chitin-based nanoparticles have recently been developed that are ex­
pected to play a significant role in anti-tumor therapy (Wan et al., 2021),
and chitin-based wound healing materials have been introduced as an
effective means of delivering drugs, regenerating damaged tissue, and
preventing bacterial activity (Baharlouei & Rahman, 2022; Li et al.,
2020; Wang et al., 2022). Comprehensive reviews of the recent advances
made in medicine can be found in the studies of Garg et al. (2019),
Jhaveri et al. (2021), Di Santo et al. (2021), Sharifi-Rad et al. (2021),
and Yanat and Schroën (2021).
Besides, chitosan nanoparticles have found practical applications in
agriculture where they have been used for the controlled release of ag­
rochemicals at desired sites (Abdel-Aziz, 2019; Fellet et al., 2021;
Muthukrishnan et al., 2019; Perez & Francois, 2016; Sharma et al.,
2019), and improving stability and reducing dosages of pesticides and
fertilizers (Kashyap et al., 2015; Pereira et al., 2019), thereby contrib­
uting to sustainable agriculture. Researchers have also reported higher
grain yield for barley and finger millet (Behboudi et al., 2018;
Sathiyabama & Manikandan, 2021). Furthermore, chitosan nano­
particles have been used in wastewater treatment as sorbents of toxic
pollutants such as heavy metals and dyes (Fan et al., 2012; Gokila et al.,
2017; Hosseini et al., 2016; Jawad et al., 2020; Lyu et al., 2019). The
high surface area of chitosan nanoparticles provides a high sorption
capacity compared to conventional sorbents (Sivakami et al., 2013). We
refer interested readers to recent reviews (Bandara et al., 2020; Brião
et al., 2020; Choudhary et al., 2019; Kashyap et al., 2015; Kasiri, 2018;
Zhang, Xu, et al., 2021; Zhang, Zhao, et al., 2021) for further informa­
tion about the application of chitosan nanoparticles in agriculture, and
wastewater treatment.
Chitin itself is often used as a base material, and there is a growing
awareness of its use in the shape of chitin nanofibers and nanocrystals,
especially for developing polymer nanocomposites. In a pioneering
study by Paillet and Dufresne (2001), chitin nanocrystals with an
average size of 150 nm (obtained via acid hydrolysis of squid pen) were
used to reinforce a latex polymer made by copolymerization of styrene
and butyl acrylate. In a follow-up study, chitin nano- and microcrystals
(average size from 500 nm up to 10 μm) obtained from Riftia pachyptila
tubes were added to polycaprolactone thus improving thermal stability

4
M. Yanat and K. Schroën Carbohydrate Polymers 312 (2023) 120789

Fig. 5. Specific strength (tensile strength/density) and specific stiffness
(Young's modulus/density) of biodegradable plastics with ChNC. The data was
compiled from (Chang et al., 2010; Colijn et al., 2022; Herrera, Roch, et al.,
2016; Oun & Rhim, 2017a; Patel et al., 2021; Ravikumar & Sagadevan, 2021;
Salaberria et al., 2014; Salaberria et al., 2017; Salaberria, Diaz, et al., 2015;
Singh et al., 2018, 2021; Zhang et al., 2014).
compared to the based polymer (Morin & Dufresne, 2002), and
encouraging further research, e.g., on natural rubber (Gopalan Nair &
Dufresne, 2003a; Gopalan Nair & Dufresne, 2003b; Gopalan Nair et al.,
2003).
Chitin nanocrystals have been incorporated mostly into PLA which is
widely considered the most promising biodegradable plastic (Broers
et al., 2018; Colijn et al., 2022; Herrera et al., 2017; Herrera, Roch, et al.,
2016; Herrera, Salaberria, et al., 2016; Singh et al., 2018, 2021, 2020;
Xu et al., 2020; Yanat et al., 2022). Moreover, PHBs (Li et al., 2021;
Zaccone et al., 2022), thermoplastic starch (Chang et al., 2010; Qin
et al., 2016; Salaberria et al., 2014; Salaberria, Diaz, et al., 2015), cel­
lulose (Oun & Rhim, 2017a, 2017b, 2020; Ravikumar & Sagadevan,
2021) and chitosan (Sun et al., 2019; C. Wu et al., 2019) films, and
others (Fernández-Marín et al., 2020; Li & Wu, 2022; Xu et al., 2019)
were explored. Addition of chitin nanocrystals to a base polymer is
mostly done to improve mechanical strength. Fig. 5 summarizes various
literature sources showing the reinforcing effect of chitin nanocrystals
both on Young's modulus and tensile strength of the composites. Low
filler loadings of chitin nanocrystals (mostly ≤5 % (w/w)) significantly
reinforced the mechanical strength. Salaberria et al. (2014) reported a
rise in Young's modulus of thermoplastic starch from 75 to 225 MPa by 5
% chitin nanocrystal incorporation. In addition, it was shown that the
glass transition temperature (Tg) of starch/ChNC nanocomposite was
improved by 7 ◦ C (Salaberria et al., 2014). Nanocrystal addition allows
efficient stress transfer from the matrix to the particles (Chavan et al.,
2022); as reflected in a prominent increase in the tensile strength of
ChNC-added nanocomposites reported by many (Oun & Rhim, 2017b;
Salaberria et al., 2014; Singh et al., 2018; Zhang et al., 2014).
Literature studies have frequently reported that nanoparticles have
the ability to decrease water vapor transfer rate (WVTR) through
biodegradable plastic composite films. Table 2 summarizes results ob­
tained for ChNC nano-particles. For 5 % chitin nanocrystals in thermo­
plastic starch, the water vapor transfer rate decreased by roughly 40 %
compared to the base material (Chang et al., 2010; Salaberria, Diaz,
et al., 2015). For PLA, ChNC addition in thin films (≤ 100 μm) improved
WVTR by around 10 % (Colijn et al., 2022; Salaberria et al., 2017)
whereas this effect reached up to ~50 % for thick films (~1 mm) (Broers
et al., 2018). The addition of 1 % ChNC to PLA/PBAT films did not result
in any improvement in WVTR (Herrera, Roch, et al., 2016). Most
probably the improved barrier function is a result of a more compact and

Table 2
The changes in water vapor transfer rate (WVTR) through biodegradable plastics due to ChNC addition.
Matrix ChNC Plasticizer WVTR Test conditions Change in Film Ref.
amount WVTR thickness

% (w/w) g⋅mm/m2 % μm
day

Thermoplastic starch 0 Glycerol (25 %) 131 ± 18a 25 ◦ C – 100 %RH – n.a. (Chang et al., 2010)
1 105 ± 9a − 19.8
2 101 ± 5a − 22.9
3 81 ± 9a − 38.2
4 79 ± 7a − 39.7
5 81 ± 7a − 38.2
Thermoplastic starch 0 Glycerol (30 %) 130 ± 0 30 ◦ C – 33 %RH – 70–72 (Salaberria, Diaz, et al.,
5 85 ± 30 − 34.6 2015)
10 80 ± 15 − 38.5
20 130 ± 15 0
PLA (60 %) PBAT (25 %) 0 Glycerol triacetate (10 5 ± 0.5 23 ◦ C – 33 %RH – 25–30 (Herrera, Roch, et al., 2016)
1 %) 5.9 ± 0.7 + 18
PLA 0 Glycerol triacetate (20 3.9 ± 1.1 20 ◦ C – 55 %RH – ~1000 (Broers et al., 2018)
0.5 %) 2.5 ± 0.1 − 35.9
1 1.9 ± 0.0 − 51.3
3 1.9 ± 0.0 − 51.3
PLA 0 Not used 38.2 ± 2.2 23 ◦ C – 85 %RH – 100 (Colijn et al., 2022)
5 35.6 ± 0.9 − 6.3 %
5b 34.6 ± 2.3 − 9.4 %
PLA 0 Not used 5.6 ± 0.1 30 ◦ C – 33 %RH – 60–100 (Salaberria et al., 2017)
0.5c 5.1 ± 0.4 − 8.9
1c 5.3 ± 0.7 − 5.4
2c 5.3 ± 0.2 − 5.4
0.5d 4.9 ± 0.1 − 12.5
1d 5.0 ± 0.2 − 10.7
2d 5.1 ± 0.2 − 8.9
a
Approximate values due to unit conversion.
b
Stearic acid-modified ChNC.
c
Acetic anhydrate-modified ChNC.
d
Dodecanoyl chloride acid-modified ChNC.

5
M. Yanat and K. Schroën Carbohydrate Polymers 312 (2023) 120789

Table 3 effect, is highly unlikely, given the three-dimensional arrangement of

The functional properties in biodegradable plastics due to ChNC addition. particles in the film, which should not increase the pathway at the low
Matrix Nano- Other Major findings Ref. particle concentrations used in these films.
particle components Although there are fewer studies on oxygen permeability than on
Thermoplastic ChNC Glycerol Antifungal (Salaberria, water vapor permeability, the findings are encouraging. For example,
starch Aspergillus niger (89 Diaz, et al., when 3 % chitin nanoparticles were added to a 51 μm thick polybutylene
% inhibition after 7 2015) succinate polymer, its oxygen permeability was reduced by 62 % (Xu
days at 25 ◦ C). et al., 2019). Similarly, in a PLA-based nanocomposite formed by the
Thermoplastic ChNC Glycerol Antibacterial (Qin et al.,
starch Listeria 2016)
same amount of ChNC, the reduction in oxygen permeability of ~50 %
monocytogenes was noted (Xu et al., 2020). According to Salaberria, Diaz, et al. (2015),
(proportional to ChNC incorporation decreased the oxygen transfer through thermo­
ChNC in film). plastic starch films by up to 25 %.
Weak or no effect
The addition of ChNC to biodegradable plastics can also provide
Escherichia coli.
PLA and PBATa ChNC Glycerol Antifungal (Herrera, them with additional functionalities, such as antimicrobial and antiox­
triacetate Aspergillus niger (70 Roch, et al., idant properties. Chitosan nanoparticles, in particular, have been used in
% inhibition after 7 2016) the medical field as antimicrobial and antioxidant agents (Landriscina
day at 25 ◦ C). et al., 2015; Sobhani et al., 2017; Vinsova & Vavrikova, 2011), and
PLA ChNCb Antifungal (Salaberria
ChNC-coated cellulose fabrics were used for filtration of water to pre­
–
Aspergillus niger et al., 2017)
(~50 % inhibition vent bacterial effects (Jalvo et al., 2021). Table 3 summarizes the effects
after 7 days at created by ChNC addition to biodegradable plastics. ChNC-containing
25 ◦ C). thermoplastic starch, PBAT, and PLA films have considerable activity
Cellulosec ChNC Antibacterial (Butchosa
–
against Aspergillus niger; one of the best-known mold food contaminants
Escherichia coli (XL- et al., 2013)
1-Blue). Log 3.0 (Salaberria, Diaz, et al., 2015; Salaberria, Labidi, & Fernandes, 2015;
reduction in viable Salaberria et al., 2017; Herrera, Roch, et al., 2016). Antibacterial ac­
cells after 3 h tivity against Listeria monocytogenes (Qin et al., 2016) and Escherichia coli
incubation. (Butchosa et al., 2013) which are important foodborne pathogens
Chitosan film ChNC Glycerol, Antioxidant (Wu et al.,
responsible for serious illness and even death, were also reported.
Curcumin activity. DPPHd 2019)
radical scavenging Furthermore, antioxidant effects can be created by addition of ChNC
activity up to 20 %, (Wu et al., 2019; Yanat et al., 2022), which reduces rancidity, and thus
and ~60 % with food deterioration and, eventually, food waste. In general, oxidation
curcumin.
reactions are initiated at the surface of the food, and antioxidants (to­
PLA ChNC – Antioxidant (Yanat et al.,
activity. DPPH 2022) copherols, plant phenolics or synthetic antioxidants) are used to miti­
radical scavenging gate this, but now, through smart package design, another option may
activity up to 33 % become a reality, which also complies with consumer preferences.
(pH 4–8). Aggregation is the main effect that hampers the application of chitin
a
Polybutylene adipate terephthalate. nanocrystals, and this has spurred interest in improving particle prop­
b
Stearic acid- or dodecanoyl chloride acid-modified ChNC. erties, such as reducing the size, also of individual nanocrystals, and
c
Bacterial cellulose nanofibers/ChNC nanocomposites. modifying the particles and their surface properties. Goodrich and
d
2,2-Diphenyl-1-picrylhydrazyl. Winter (2007) found a specific surface area of chitin nanocrystals of 347
m2 per 1 g. Highly crystalline and thermally stable (up to 250 ◦ C)
tightly packed polymer structure that is induced by the presence of the α-chitin nanocrystals were prepared (Sriupayo et al., 2005) using the
particles, and that reduces diffusion (Colijn, 2023). In our opinion, the TEMPO-mediated oxidation method (Fan et al., 2008, 2009). Surface
claim often made that a longer diffusion pathway is responsible for this modification to tune the hydrophobicity of the particles was reported,

Fig. 6. Common modification routes of chitin-based materials.

6
M. Yanat and K. Schroën
and successfully applied to reduce aggregation (Dufresne, 2008) and
improve dispersion in PLA films (Colijn et al., 2022).
Ideally, nanocrystals should form a percolation network within the
polymer matrix through strong hydrogen bonds (Mariano et al., 2014);
however, there is a compatibility issue between the relatively hydro­
phobic biodegradable plastics and the hydrophilic backbone of ChNC
(also for other polysaccharide-based NPs). Researchers have tackled this
issue identifying aggregation strength of nanocrystals. In the work of
Colijn et al. (2021) a minimum energy input of ~100 kJ/g was found for
ultrasound treatment to break up chitin nanocrystal aggregates.
As mentioned, surface modification of particles through chemical
grafting has been used to improve dispersibility (Fig. 6 shows common
modification routes of chitin-based materials). This involves the reactive
hydroxyl, acetamide, and amine groups on the nanoparticle surface. The
most straightforward modification method is by deacetylation, which
converts acetamide groups to amine groups, resulting in a more posi­
tively charged surface that in turn opens new routes for further modi­
fication. Alkylation or quaternization at the amino group at the C2
position (Muñoz-Núñez et al., 2022), or carboxymethylation (Ma et al.,
2008), all lead to more hydrophilic particles that are advantageous for
biomedical applications, but not for biodegradable plastics that require
more hydrophobic particles. The hydroxyl groups can be used to intro­
duce hydrophobic groups and thus reduce surface energy (Huang et al.,
2015). Surface acetylation was used to functionalize particles by reac­
tion with acetic anhydride leading to improved PLA nanocomposites
(Zhang et al., 2014). The addition of 4 % of these acetylated chitin
nanocrystals improved the tensile strength and Young's modulus by 45
and 37 %, respectively, compared to neat PLA films. Furthermore,
modification with e.g., fatty acids and silane coupling agents were
shown to boost chemical bonding between chitin nanocrystals and
biodegradable plastics (Colijn et al., 2022; Li et al., 2021). Improved
phase compatibility between PHB and amino silane coupled-ChNC has
also been reported (Li et al., 2021).
Melt mixing (or melt compounding) and solution casting are the
main preparation methods. The latter is preferred in a lab-setting, and
uses the dissolution of polymer in a solvent (mostly chloroform) and
adding nanocrystals dispersed in the same or different solvent. It is
worth noting that this allows formation of large and strong aggregates
due to the duration of this process. On a larger scale, extrusion is
employed to create nanocomposites via melt mixing ideally leading to
de-aggregation of chitin nanocrystals through mechanical shearing ac­
tion in the molten polymer matrix. Extrusion has been shown to improve
the dispersibility of ChNC in biodegradable polymers (Herrera, Roch,
et al., 2016; Li et al., 2017; Rizvi et al., 2011; Salaberria et al., 2014; Wu
et al., 2008); although it is good to point out that the ~100 kJ/g
mentioned earlier is not that easy to achieve. In general, dispersing
agents, also known as plasticizers such as triethyl citrate (TEC) and
glycerol triacetate (GTA), are used, and have been shown to enhance the
flexibility and transparency of resulting nanocomposites (Herrera et al.,
2017; Patel et al., 2021, 2022), although often at the expense of tensile
strength and storage modulus. In that respect, particle modification can
result in dual beneficial effects; it will improve compatibility between
polymer and particle, thus reducing aggregation, and contributing to
percolated network formation that is expected to improve the mechan­
ical strength of the nanocomposites. The whole range of modification
methods that can be applied to chitin/chitosan puts them at the fore­
front for various applications.
4. Conclusion and outlook
To reduce our dependency on non-renewable sources, bio-based
packaging materials need to be developed. Chitin-based nanoparticles
not only have been proposed to enhance the mechanical strength and
thermal stability of packaging materials, but also to facilitate adding
new functionality (antibacterial, antioxidant). At present, chitin
nanocrystal-reinforced biodegradable plastics (especially ChNC/PLA)
7
Carbohydrate Polymers 312 (2023) 120789
have comparable or even better water vapor and oxygen permeability
properties than common petroleum-based plastics (polyethylene and
polystyrene), but are not yet at the level of PET.
Overall, the future of biobased, and biodegradable plastics is looking
bright and chitin nanocrystals can have an essential role in this,
although it is good to point out that the dispersion of these nanoparticles
is a critical factor. Fortunately, this can be addressed through surface
modification for which chitin-based particles hold ample opportunities.
CRediT authorship contribution statement
Murat Yanat: Conceptualization, Writing - original draft, review &
editing, Visualization.
Karin Schroën: Writing - review & editing, Supervision, Funding
acquisition.
Declaration of competing interest
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.
Data availability
Data will be made available on request.
Acknowledgements
This work was carried out under project number A17020 as part of
the research program of the Materials Innovation Institute (M2i), which
is supported by the Dutch government. Funding for this research was
obtained from Yparex, Oerlemans Packaging B.V., Koninklijke Peijnen­
burg B.V., Heineken, and Jacobs Douwe Egberts. The authors are
thankful for the financial support for the PhD training of Murat Yanat by
the Republic of Turkey Ministry of National Education.
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