Amounts (g and wt %) of chitosan (CS), glycerol (G), bentonite (BNT), used for the preparation of chitosan, chitosan/glycerol, chitosan/BNT, and chitosan/glycerol/BNT.
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The increase in living standards, changing consumer habits, and industrial development led to a high consumption of biodegradable plastic materials [1]. One of the best options to reduce current packaging waste is the use of biodegradable films that allow the final replacement of plastic packaging bags which are not recycled and are thus a pollution source. The present research is directed toward the development of biodegradable ecofriendly materials with enhanced properties [2]. Chitosan (CS) is a deacetylated derivative of chitin, which is the most abundant polysaccharide in nature after cellulose; it is a natural polysaccharide, biocompatible, and biodegradable in addition to the antibacterial properties that can be useful in many areas as the food packaging industry. Chitosan which consists of a linear (1–4) linked 2-amino-2-deoxy-D glucan as shown in Figure 1 is a relatively inexpensive material, next to cellulose.
Chemical structure of Chitosan.
Chitin and chitosan are biopolymers having immense structural possibilities for chemical and mechanical modifications to generate novel properties, functions, and applications [3, 4], as biomedicine [5, 6], pharmaceuticals [7, 8, 9], metal chelation [10, 11], and food additives [12] and in the fabrication of sensors or biosensors [13].
Chitosan is highly soluble in acid aqueous solution. The positive charge and molecular arrangement confer to chitosan’s interesting properties [14]. Figures 2 and 3 illustrate the protonation of chitosan which leads to soluble material. Figure 4 shows the simulation of protonated chitosan backbone (positive charges of NH3+ onto chitosan polymer) in acid aqueous solution. These positive charges cause a mutual repulsion and thus a swelling behavior and good solubility of chitosan. The protonation constants pKa of chitosan decrease slightly, from 6.3 when the molecular weight reduces. The degree of deacetylation effects on pKa values. The decrease in degree of deacetylation increases the pKa. The degree of deacetylation influenced the balance of hydrophobic interactions and hydrogen bondings on chitosan [15].
Protonation of chitosan in acetic acid aqueous solution.
Polymer backbone of protonated chitosan in acid aqueous solution.
Simulation of protonated chitosan backbone in acid aqueous solution.
In the same way, bentonite clays are also abundant and low-cost natural materials. Sodium bentonite is the name for the ore whose major constituent is the mineral, sodium montmorillonite. Montmorillonite is a three-layer mineral consisting of two tetrahedral layers sandwiched around a central octahedral layer. Bentonite is rich in montmorillonite (usually more than 80%) [16, 17, 18, 19]. Bentonite and montmorillonite names are often used interchangeably. However, the terms represent materials with different degrees of purity. Bentonite is the ore that comprises montmorillonite, inessential minerals, and other impurities.
When sodium bentonite comes into contact with water, the atoms and molecules dissolve, and ions with negative charges develop. These negative charges cause a mutual repulsion and thus a swelling within the clay structure. Figure 5 shows the three-layer structure of a particle of bentonite and its exfoliation in sodium hydroxide aqueous solution.
The three sheet structure of a particle of bentonite.
The cations residing between the layers of sodium bentonite (Na-BNT or simply BNT) are exchangeable with ammonium ions of chitosan. This process converts the hydrophilic surface of the layer into a hydrophobic one, thereby improving the compatibility of nanoclay into polymer matrix.
The three processes that may occur in chitosan polymer and clay mixture, as shown in Figure 6, are intercalation, exfoliation, and conventional distribution. Intercalation is a physical process by which a macromolecule like a polymer is inserted in the clay sheets. Such a molecule is flanked by two clay layers and is immobilized and shielded. Exfoliation is a delaminating process wherein the gallery is expanded from its normal size of 1 nm to about 20 nm or higher. Thus there is a clear disruption of the layers which get spatially separated apart bringing about nanoscale dispersion in the polymer matrix. Thus exfoliated clays represent true nanomaterials. Intercalation and exfoliation of the clays can be accomplished using polymer from its solution or a melt [20].
The three processes that may occur in polymer and clay mixture.
Chitosan/bentonite composites are economically interesting because they are easy to prepare and involve inexpensive chemical reagents. Nanocomposites prepared from chitosan/bentonite shape natural films with a great potential and provide physical protection, they are biocompatible and biologically active toward microbial growth while being nontoxic and biodegradable. These nanobiocomposites obtained by adding nanofillers to biopolymers like chitosan result in very promising materials since they show improved properties with preservation of the material biodegradability without eco-toxicity [21].
Although chitosan/clay nanocomposites are very interesting materials, they were not extensively investigated as potential film packaging for food application. Thus, the aim of this work is to analyze the role of the chitosan/bentonite ratio, the DDA of chitosan, and a plasticizer specially glycerol in the solution casting process for the achievement of chitosan/clay nanocomposite films. In order to investigate the combined effect of glycerol and unmodified clay on the properties of chitosan-based nanocomposites, films containing different amounts of clay and glycerol were prepared and characterized with particular regard to structural, thermal, and mechanical properties. Finally, new nanocomposite active films were proposed for safe packaging of edibles [22].
Chitosan (CS) with different degree of deacetylation (DDA) (from 70 to 100%) in powder form was prepared in our laboratory from exoskeletons of shrimp waste and purified [23, 24]. The chitosan chemical structure is schematically shown in Figure 1. The degree of deacetylation (DDA %) was determined by conductimetric titration [20].
Analytical grade sodium periodate ACS reagent, 99.8–100% dry basis, and bentonite were purchased from Sigma-Aldrich. Sodium bentonite used in this study was purified according to the method reported by H. Sedighi et al. [25]. The bentonite ore was beneficiated to improve its montmorillonite content by removing the impurities, generally albite, calcite, dolomite, orthoclase cristobalite, and quartz. The crude sample was primarily crushed at the size of 2 mm, and 5 g of bentonite powder was added to 100 mL of hot deionized water and stirred for 2 h. The separation of the impurities is obtained by a sedimentation process of the solution. The settled precipitate is mostly impurities, and the solid collected from the supernatant is generally pure montmorillonite. The slurry and solid phases were separated by filtration, and the remaining solid was dried at 150°C. All the other chemicals used are of analytical grade and used as received.
Chitosan solution was prepared by dissolving 1 g of chitosan powder in 100 ml of aqueous acetic acid solution (1%, v/v), under continuous stirring at room temperature for 2 h followed by vacuum filtering to remove the insoluble residue. This solution was cast into Petri dishes and dried at 50°C for 20 h to evaporate the solvent and form the films. The dried films were soaked with an aqueous solution of 0.05 M NaOH to remove residual acetic acid, followed by rinsing with distilled water to neutralize, and then dried at room temperature.
Chitosan/Na-BNT (also described as CSBNT) films were prepared using the casting/solvent evaporation technique. Firstly, 1% chitosan solutions were prepared by dissolving 1 g of chitosan powder in 100 ml of aqueous acetic acid solution (1%, v/v), under continuous stirring at room temperature for 2 h followed by vacuum filtering to remove the insoluble residue. Nanocomposite samples were obtained by dispersing selected amounts of bentonite in aqueous solution and stirred at 50°C until swelling was completed. After, the dispersion was slowly added to the CS solution to reach a final clay concentration of 1, 2, 3, and 5 wt% followed by stirring at room temperature for 5 h and then for 30 min at 25°C in ultrasonic bath. The amounts of chitosan, clay, and plasticizer used for each sample are listed in Table 1. For example, the composite film CSBNT1% is 1% BNT and 99% CS prepared from 1 g chitosan and 0.0101 g bentonite.
Sample | Chitosan (g)-wt% | BNT (g)-wt% | Glycerol (g)-wt% |
---|---|---|---|
CS | 1–100% | — | — |
CSBNT1% | 1–99% | 1% | — |
CSBNT2% | 1–98% | 2% | — |
CSBNT3% | 1–97% | 3% | — |
CSBNT5% | 1–95% | 5% | — |
CSG | 1–70% | — | 30% |
CSGBNT1% | 1–69% | 1% | 30% |
CSGBNT2% | 1–68% | 2% | 30% |
CSGBNT3% | 1–67% | 3% | 30% |
CSGBNT5% | 1–65% | 5% | 30% |
Amounts (g and wt %) of chitosan (CS), glycerol (G), bentonite (BNT), used for the preparation of chitosan, chitosan/glycerol, chitosan/BNT, and chitosan/glycerol/BNT.
CS: Chitosan, BNT: bentonite, CSBNT1%: Film chitosan/bentonite 1%, CSBNT2%: Film chitosan/bentonite 2%, CSBNT3%: Film chitosan/bentonite 3%, CSBNT5%: Film chitosan/bentonite 5%, CSG: Film Chitosan/Glycerol, CSGBNT1%: Film Chitosan/Glycerol/bentonite 1%, CSGBNT2%: Film Chitosan/Glycerol/bentonite 2%, CSGBNT3%: Film Chitosan/Glycerol/bentonite 3%, CSGBNT5%: Film Chitosan/Glycerol/bentonite 5%.
The nanocomposite solutions were then poured into Petri dishes and dried at 50°C for 20 h to evaporate the solvent and form the films. Free chitosan and nanocomposite films plasticized with glycerol were obtained by adding glycerol (30% (wt/wt) on solid CS) to the CS solution while stirring for 20 min at room temperature.
Following the same procedure used for chitosan films, the dried films were soaked with an aqueous solution of 0.05 M NaOH to remove residual acetic acid, followed by rinsing with distilled water to neutralize, and then dried at room temperature.
Chitosan/Na-BNT/cross-linker films were prepared using same method of manufacturing of chitosan/Na-BNT films. The dialdehyde chitosan was used as cross-linker and prepared according to I. Charhouf et al. [26] method and added after dispersing BNT in CS solution.
Mix 1 g chitosan ([CS] = 5.34 mM) in suspension with 50 ml HCl (10−3 M) (pH ranging from 4 to 5) with magnetic stirring. Mix with 1 ml aqueous solution of sodium periodate 0.534 mM, P0 = 0.1 (P0 = moles of NaIO4 x moles of CS). The reaction was carried out at 4°C in the dark for 30 minutes. After reaction, to eliminate the unreacted periodate, add 1 ml ethylene glycol. The oxidized chitosan was washed by distilled water for 4 h and freeze-dried.
The oxidation of chitosan using NaIO4 was well characterized as reported by I. Charhouf et al. [26]. In this work, we partially oxidized chitosan with a very few amount of sodium periodate. It is clearly seen from Figure 7 that the oxidation reaction leads to opened structure of chitosan with dialdehyde functions.
Oxidation reaction of chitosan by sodium periodate.
Fourier transforms infrared (FTIR) spectra of the chitosan films and the chitosan/clay films were collected using a Tensor 37 FT-IR spectrophotometer (Spectrum 400 Perkin Elmer) operating in the range of 400–4000 cm−1 at a resolution of 4 cm−1.
Mechanical properties of chitosan/clay nanocomposite were measured with a Universal Testing Machine Ludwig mpK, tensile strength (TS), and percentage elongation at break (EL) of the films at 25°C according to ASTM D882 standard procedures [27]. The films were cut to a dog bone shape with a rectangular midsection (100 mm long x15 mm wide) flaring to 25 mm x 35 mm sections on each end. The thickness of each sample was measured with micrometer at three different locations and averaged. The films were conditioned at 50% RH for 72 h before each test. A 100 N load cell was used and the extension rate was set at 5 mm/min [28].
The tensile strength (σ) and percentage of elongation at break (E) were calculated using the following equations:
where F maxis the maximum load (N), A is the initial cross-sectional area (m2), ∆l is the extension of film strips (m), and L0 is the initial length (m).
The thermal properties of nanocomposites and pure chitosan were investigated by thermogravimetric analysis (TGA). Samples were placed in the balance system and heated from 25 to 600°C at a heating rate of 10°C/min under a nitrogen atmosphere. Three replicates were tested for each sample.
The X-ray diffraction analysis of the obtained films was performed by diffractometer with Cu Kα radiation (λ = 1.5418 A°) at room temperature. XRD scans were performed on sodium bentonite, chitosan films, and chitosan/bentonite films with a 2θ range between 5°-30°, at a scanning rate of 1°/min and scanning step of 0.01°.
Conventional high-vacuum scanning electron microscopy (SEM) images were also taken to visualize the structure of chitosan and oxidized chitosan. Chitosan and oxidized chitosan were freeze and dried for 24 h and were sprayed on silicon wafer substrate, then sputter-coated with gold (Agar Manual Sputter Coater; Marivac Inc., Montreal, QC, Canada), and imaged using a Quanta 200 FEG Environmental Scanning Electron Microscope (FEI Inc., Hillsboro, OR). Observations were performed at 20 kV using the high-vacuum mode.
The microstructural characterization of nanocomposites was carried out on the following samples: CSBNT3%, chitosan/bentonite 3%; CSBNT5%, chitosan/bentonite 5%; CSBNT10%, chitosan/bentonite 10%; CSBNT20%, chitosan/bentonite 20%; and CSG, chitosan/glycerol. Samples in powder form were coated in epoxy and ultramicrotomed with a diamond knife at -100°C. The recovered thin sections were observed at transmission electron microscope (TEM) (JEOL 2011) operating at 200 kV and the remaining blocks at field emission gun scanning electron microscope (FEGSEM) (Hitachi S 4700) at 1 kV after a slight platinum metal deposition.
The intercalation of the cationic biopolymer chitosan into layered silicate clay (bentonite) through a cation exchange process results in nanocomposites with interesting structural and functional properties. Chitosan/Na-BNT films were prepared using the same method of manufacturing of chitosan films. However, Na-BNT was exfoliated in sodium hydroxide aqueous solution, purified, and washed prior to be added to chitosan solution. Organic matter is present in bentonite as intrinsic impurities composed predominantly of humid substances. Since competitive reactions can take place between the organic matter present in the bentonite and the chitosan, the extent of intercalation and polymer/clay interactions can be affected. Purification capable of removing of organic matter from bentonite before intercalation is fundamental.
The plasticization action of water molecules on hydrocolloid-based films has been widely reported in the literature [29, 31, 32]. In addition to water, the most commonly used plasticizer was glycerol (G), thus nearly systematically incorporated in most of biopolymer films [30]. Glycerol is indeed a highly hygroscopic molecule generally added to film-forming solutions to prevent film brittleness [31, 32]. The interest in use of the glycerol is that it acts as plasticizer and reduces the intermolecular forces by increasing the mobility of the biopolymer chains. The glycerol reduces the extent interactions between Na-BNT stacks making it possible to achieve a better dispersion of nano-sized filler and can modify the ability of water to swell BNT in the aqueous solution, due to the ability to reduce the surface energy of aqueous solution.
In this study as shown in Figure 8, chitosan (CS)/(BNT) nanobiocomposite and chitosan (CS)/(BNT)/cross-linker films were prepared by the intercalation of chitosan in bentonite to form miscible, biodegradable nanocomposite material used as packaging films for food preservation.
The sheets structure of exfoliated bentonite and dispersed in crosslinked chitosan matrix.
Periodate oxidation of chitosan have been relatively little explored, with only a few studies on the periodate oxidation reaction and products formed. Recently, Charhouf et al. [33] studied the periodate oxidation and the physical characterization of oxidized chitosan more in detail. The periodate oxidation of chitosan obviously leads to changes in the chemical structure. The cleavage of C2–C3 in chitosan (CS) units leads to the formation of a dialdehyde. Reaction of cross-linking chitosan and dialdehyde chitosan takes place when dialdehyde group reacts with amine moiety of unmodified chitosan as shown in Figure 9 giving a cross-linked material.
Crosslinking reaction between chitosan and dialdehyde chitosan.
The nanocomposite films prepared by casting technique using two inexpensive resources available and biocompatible (chitosan and Na-bentonite) were obtained as shown in Figure 10.
Images of chitosan/bentonite nanocomposite films casted from solutions containing chitosan (2% w/w) and bentonite at various amount of pure clay.
The presence of a group like hydroxyl, on the surface of chitosan, facilitates encapsulation of essential oils (EOs) or bioactive compound. The nanoemulsions were used to stabilize the EOs in the chitosan matrix, without altering its film-forming properties [34]. We investigated different emulsion formulations to encapsulate essential oils and to study their effects on the in vitro antimicrobial activity against various microorganisms. Figure 11 shows images of antimicrobial films casted from solutions containing modified chitosan (2% w/w), dyes, and essential oils (0.05% w/w).
Images of antimicrobial films casted from solutions containing modified chitosan (2% w/w) and essential oils (0.05% w/w) added as pure rosemary essential oil.
Rosemary essential oil, with its warm and penetrating aroma, is one of the most stimulating oils used in aromatherapy. Rosemary was one of the earliest plants to be used in medicine, as well as for cooking. It has a very strong antiseptic action so it is terrific to use in aromatherapy recipes for cleaning. Incorporation of essential oils (EOs) in chitosan films was studied in order to prepare antimicrobial barriers to be applied to food surfaces. Essential oils were directly incorporated in the chitosan nanocomposite matrix. The EOs were selected by their ability to develop antimicrobial synergies against Listeria bacteria (monocytogenes or innocua) with chitosan, which is characterized by intrinsic antimicrobial properties.
FTIR spectra of chitosan (CS), bentonite (BNT), and chitosan/bentonite nanocomposite (CSBNT) films are displayed in Figure 12. The spectrum of chitosan shows a broad peak at 3475.80 cm−1 corresponding to amine N–H symmetrical vibration and H bonded O–H group; the peaks at 2924.44 cm−1 were assigned to the symmetric and asymmetric –CH2 vibrations of carbohydrate ring. The absorption peak observed at 1618.79 cm−1 was assigned to (C = O in amide group, amide I vibration), 1545 cm−1 was attributed to (–NH2 bending of amide II), and 1390 cm−1 was given to (N–H stretching or C–N bond stretching vibrations, amide III vibration). The peak at 1116.93 cm−1 corresponds to the symmetric stretching of C–O–C groups. The absorption peaks in the range 900–1200 cm−1 are due to the antisymmetric C–O stretching of saccharide structure of chitosan.
FTIR spectrum of: Chitosan film (FCSBNT0%), Chitosan/BNT films respectively (FCSBNT3%) and (FCSBNT5%).
As can be seen in Figure 12, the FTIR spectrum of BNT shows a peak at 1010 cm−1 that belongs to Si-O-Si linkage. In addition, the characteristic absorption peaks are found at around 3670 cm−1 (stretching vibration of Al-OH and OH), at 3465 cm−1 (stretching vibration of O-H and H-O-H groups), at 1638 cm−1 (H-O-H bending vibration), at 933 cm−1 (Al-Al-OH bending frequency), and at 509 cm−1 (bending vibration of Si-O).
The FTIR was also used to study the polymer/clay interaction, since a shift in the NH3+ vibration may be expected when – NH3+ groups interact electrostatically with the negatively charged sites of the clay [35]. Nevertheless, this shift is higher for CSBNT nanocomposite film with the lowest amounts of CS, while the chitosan/clay films with the highest amounts of biopolymer show a frequency value that trends to that observed in the films of pure chitosan (CS). This fact may be related to the –NH3+ groups that do not interact electrostatically with the clay substrate. The spectrum of CBNT nanocomposite film (Figure 12) shows a characteristic band at 3462.78 cm−1 attributed to hydrogen bonding formation due to the functional groups of CS (O-H and N-H groups) and BN (O-H groups) [36, 37]. The intensity of the NH3+ band also increases for higher amounts of intercalated chitosan. The secondary amide band at 1645 cm−1 of chitosan is overlapped with the HOH bending vibration band at 1628 cm−1 of the water molecules associated to the chitosan/clay films, which are present as in the starting clay, as expected for a biopolymer with high water retention capability [38, 39].
The stress-strain curves of the tested specimens are being presented in Figure 13, while the average values along with the standard deviation of Young’s modulus, tensile strength and elongation at break of the films on the stress-strain behavior of the chitosan and chitosan/glycerol films, respectively [40], are shown in Figure 14. The higher strength obtained in the case of the CS films can be attributed to more efficient stress transfer between the adjacent chains due to the strong electrostatic interactions between the NH2 and NH3+ groups. The CSG specimen presents almost double strength (at yield and break) and elongation at break. Due to the lower acidity of the diluted films, a weaker hydrogen bond network was established between the amino groups and the glycerol chains. On the other hand, the extensive deformation strengthening in undiluted systems (CSG) suggests the creation of a long-range order and the formation of hydrogen bonding after the addition of glycerol.
Stress-strain curves of chitosan film (FCSBNT0%), chitosan/BNT films (FCSBNT3%), (FCSBNT5%), respectively.
The effect of BNT addition on the tensile response of the chitosan and chitosan/glycerol films is being depicted. The stress–strain curves of BNT composite films prepared from the 1 w/v% chitosan solution is being presented. The addition of BNT results in a pronounced enhancement of the stiffness and a dramatic decrease in the elongation at break of all clay-added systems. Further addition of BNT leads in intercalated structures which limited the polymer-clay interactions and thus their reinforcing ability.
The results on mechanical properties showed the increase in the tensile strength (TS) and elastic modulus (EM) of such nanocomposite films can be attributed to the high rigidity and aspect ratio of the nanoclay as well as the high affinity between the chitosan and the bentonite. On the other hand, the CS/BNT nanocomposites have shown significant decrease in elongation at break (EB). This reduction can be attributed to the restricted mobility of macromolecular chains.
In Figure 14, effect of BNT addition is being illustrated for the diluted systems (CS nanocomposites). The ductile response of the CS films is maintained after the addition of BNT with strength and a relative lower decrease in the elongation at break. The systems with 3 wt% BNT presented the lowest enhancement in all mechanical properties.
Mechanical properties of chitosan/BNT particles films. Chitosan film (FCSBNT0%), chitosan/BNT films (FCSBNT3%), (FCSBNT5%), respectively, and chitosan/glycerol film (FCSGBNT0%), chitosan/glycerol/BNT films (FCSGBNT3%), (FCSGBNT5%), respectively.
Figures 13 and 14 present the combined effect of glycerol and BNT on the tensile response of the CS-based nanocomposites. The first observation is that the addition of BNT results in a direct reduction of the strength of the chitosan/glycerol. A completely different stress–strain behavior is being obtained after the addition of BNT in diluted chitosan/glycerol systems (Figure 14). The CS/glycerol-based nanocomposites behave like hyperelastic materials rather than like ductile polymers. It is assumed that more water and glycerol are distributed in the chitosan network, inducing a very obvious plasticization effect. The extent of hydrated chitosan crystals was confirmed from the intensities of the XRD patterns. It is very interesting to note that although the mechanical properties of the unreinforced chitosan are comparable before and after the application of the reflux processing, reflux resulted in a fourfold increase of the stiffness and strength of the nanocomposite films.
The thermal stability of the chitosan (CS) and its nanocomposites has been investigated by TGA under nitrogen (Figure 15). There are two steps of degradation. The first range (50–200°C) is associated with the loss of water, whereas the second range at 270°C corresponds to the deacetylation and degradation of chitosan, and the third step, in the temperature range 450–550°C, can be associated with the oxidative degradation of the carbonaceous residue formed during the second step.
Thermal properties of: Chitosan (FCSBNT0%) and Chitosan/Bentonite films (FCSBNT3%), (FCSBNT5%).
The nano-dispersed clay in the chitosan matrix exhibits a significant delay in weight loss. The nanocomposite forms char with a multilayered carbonaceous-silicate structure, which may keep its multilayered structure in the polymer matrix. This high-performance carbonaceous-silicate char builds up on the surface during burning, thus insulating the underlying material and slowing the escape of the volatile products generated during decomposition. The decomposition temperature CS/BNT nanocomposites show higher thermal stability than those of the pure CS. The thermal stability of the nanocomposites increases systematically with increasing clay.
For nanocomposites containing glycerol, a further degradation step at T≈250°C is observed, related to the loss of unbound glycerol, as indicated in Figure 16. Furthermore, it can also be observed that the presence of glycerol plasticizer increases of about 20°C the degradation temperature for the third step, irrespective of the presence or not of the clay.
Thermal properties of: Chitosan/Glycerol (FCSG), Chitosan/Glycerol (FCSGBNT0%) and Chitosan/Glycerol/Bentonite (FCSGBNT3%) and (FCSGBNT5%) films.
The XRD patterns of chitosan and chitosan-based nanocomposite films in the range of 5–30° are shown in (Figure 17). The basal plane of BNT shows a reflection peak at about 2θ = 8.8°. After incorporating BNT within CS, with CS/BNT, the basal plane of BNT at 2θ = 8.8° disappears, substituted by a new weakened broad peak at around 2θ = 12.8°–13.0° (CSBNT3%, CSBNT5%). It is suggested that the BNT form intercalated and flocculated structures.
XRD patterns of: Chitosan (CS), Bentonite (BNT) and Chitosan/Bentonite films (FCSBNT3%) and (FCSBNT5%).
On the base of XRD patterns, it is suggested that the BNT forms intercalated and exfoliated structures at higher CS content (CSBNT5%), while decreasing the CS content (CSBNT3%), clay layers (BNT) form intercalated and flocculated structures. According to [23], the formation of flocculated structure in CS/clay nanocomposites can be due to the hydroxylated edge-edge interactions of the clay layers. Since one chitosan unit possesses one amino and two hydroxyl functional groups, these groups can form hydrogen bonds with the clay hydroxyl edge groups. This strong interaction is believed to be the main driving force for the assembly of BNT in the CS matrix to form flocculated structures.
The XRD patterns of chitosan/glycerol films obtained from 30 w/v% solutions are shown in Figure 18. The addition of glycerol results in a pronounced peak at 12.5°. Because of the hydrophilic and polycationic nature of chitosan in acidic media, this biopolymer has good miscibility which is attributed to the interaction of glycerol molecules with chitosan macromolecules. Glycerol favors the chains mobility and thus the chitosan crystallization process in the early stage of the post-processing aging the effect of glycerol addition. The XRD patterns of chitosan/glycerol/BNT films obtained from chitosan solution are shown in Figure 18. The combined addition of glycerol and clays resulted in great enhancement of the chitosan crystallinity of the nanocomposite films prepared with 1 w/v% chitosan solution. This indicates that the presence of clay facilitates the distribution of glycerol within the chitosan matrix and the interaction of glycerol molecules with chitosan macromolecules. The combined addition of glycerol and clay had an opposite effect in films obtained from low content chitosan solution leading to decrease of the XRD peaks intensities. In addition a new peak at 18.2° appeared in XRD patterns of all obtained films. This diffraction peak is characteristic for chitosan films prepared using acetic acid solution as solvent.
XRD patterns of: Chitosan (CS), Bentonite (BNT), Chitosan/Glycerol (FCSG) and Chitosan/Glycerol/Bentonite films (FCSGBNT3%) and (FCSGBNT5%).
The addition of glycerol favors the opening of the clay galleries resulting in intercalated nanocomposites in comparison to samples without glycerol.
Chitosan/Na-BNT nanocomposites exhibit an intercalated or intercalated/orientated structure of clays. In particular, the X-ray diffraction results show that in film without glycerol, the BNT stacks lay with their platelet surface parallel to the casting surface. The presence of glycerol, on the other hand, enhances the chitosan intercalation in the silicate galleries and hinders the flocculation process, leaving the BNT stacks randomly orientated in the space.
The SEM images of chitosan and oxidized chitosan at high vacuum and at different magnifications are shown in Figure 19, showing that there is no change of elongated and fibrous network of chitosan, but on the surface of oxidized chitosan, we can see a slight degradation of some leaves.
SEM images of (a & b) chitosan and (c & d) oxidized chitosan at different magnifications.
We present in this study the microstructural characterization results obtained on the chitosan/Na-BNT nanocomposites too. The dispersion and the exfoliation of the clay were observed at field emission gun scanning electron microscope (FEGSEM) and transmission electron microscopy (TEM).
The results of the observation of the microtome block of chitosan/bentonite (CSBNT3%) and (CSBNT5%) samples are presented in Figure 20.
Images of FEGSEM of chitosan/BNT 3%.
At low magnification, the CSBNT 3% powders were observed, and clusters were found grouped into in the epoxy more matte and dark appearance (Figure 20a). Decohesion between the epoxy and the sample powders is visible in greater or lesser proportion, probably due to preparation and cutting. At higher magnification, small clay particles of a few hundred nanometers are observed, which are relatively well dispersed in the polysaccharide (Figure 20b). However, a large clay aggregate of about 10 microns was also observed (Figure 20c and d).
At higher magnification, small clay particles similar in size to those observed in the CSBNT 3% sample are regularly observed with chitosan/BNT 5% as shown in Figure 21.
Image of FEGSEM of chitosan/BNT 5%.
Transmission electron microscopy (TEM) images indicated that the silicate layers were dispersed in the chitosan matrix. The results of the TEM observation of the chitosan/BNT 3% sample show that small particles of clay from less than 100 nanometers to a few hundred nanometers are observed at low magnification which is consistent with the FEGSEM observations. Larger aggregates of clay are also observed but more rarely.
Depending on the level of the clay particles, the leaflets are sometimes well aligned (Figure 22) and sometimes of more unstructured appearance (Figure 23). This unstructured aspect of the clay sheets may be a sign of a more advanced level of intercalation. There are also some isolated single or double leaflets around other clay particles (Figure 23), which is a clear sign of exfoliation.
Images TEM of chitosan/BNT 3% (x 500K).
Images TEM of chitosan/BNT 3% (x 600K).
As expected, the concentration of clay in the polysaccharide affects the dispersion of the clay. The higher the concentration, the poorer the dispersion is obtained which is the effect of the greater aggregation of the clay. A good but not always uniform dispersion is observed in chitosan/BNT 3% and 5%. Similarly, the concentration of clay also appears to affect the level of intercalation/exfoliation. Based on MET observations, signs of exfoliation (the presence of isolated single or double clay leaflets and more unstructured appearance of the leaflets in the particles) are visible in samples of lower clay concentration less than 10%.
Natural biopolymer-based biodegradable packaging materials are a new generation of polymers emerging on the packaging market, and driven by the perception that biodegradable plastics are “environmentally friendly,” their use is predicted to increase chitosan, a natural material that has interesting antimicrobial and film-forming activities. Its application in films can contribute to food preservation and shelf-life extension. In this study, various films were successfully prepared by the solution casting technique and characterized with particular regard to structural, thermal, and mechanical properties. Films of chitosan/bentonite, chitosan/glycerol/bentonite, and chitosan/glycerol/bentonite/essential oil nanocomposites were prepared with purified bentonite (BNT), and according to the process used, they might be less expensive than other packaging materials.
Exfoliated chitosan/clay nanocomposites of varying clay contents have been successfully prepared with or without the presence of glycerol (plasticizer) and oxidized chitosan (cross-linker). This approach represents a new route to prepare high-performance nanocomposite materials. The oxidized chitosan could partially react with the amine groups on chitosan; as a result, high mechanical properties can be obtained. The Na-BNT layers are exfoliated by chitosan chains and disorderly dispersed in the chitosan matrix, as confirmed by XRD and TEM characterization. The incorporation of a small amount of clay into the chitosan matrix results in obvious enhancement in the thermal properties of chitosan. The chitosan/clay nanocomposites retain good mechanical properties. Once the clay is exfoliated and efficiently dispersed into the chitosan matrix, the storage modulus and tensile property of the chitosan/clay nanocomposites are significantly improved with respect to that of neat chitosan.
This work would not have been possible without the great support of Julian Zhu, a polymer chemist professor at Montreal University, Department of chemistry, Quebec, Canada. This work was supported by the Francophone University Association (AUF).
In the last decade, there had been a rapid change in the dietary lifestyle among the world populace owing to increased globalization, urbanization and rapid economic development [1]. The rapid changes had also resulted in a large number of people suffering from poor health conditions due to the food they consume. Owing to this, there had been an increase in people’s awareness about the role in which foods play in the emergence of these diseases [2, 3, 4]. One of such diseases resulting from food consumption is celiac disease (CD). Celiac disease, an autoimmune disorder, triggers when a genetically pre-disposed person or individual is exposed to dietary gluten resulting in the inflammation or damage of the lining of the small intestine. Celiac disease had become a global health challenge in which its prevalence is approximately 1% of the total world population with variation among regions, age, and sex [5]. However, there had been an increase in the prevalence of celiac disease in the US; a reason which was unclear but attributed to environmental component of celiac disease such as changes in the pattern of feeding, quality of ingested gluten, the spectrum of gastrointestinal infestation as well as the colonization of the gut microbiota. Symptoms associated with individuals suffering from celiac disease include retardation of growth, malnutrition, anemia, diarrhea as well as fatigue [6]. Currently, the only proven remedy for the treatment of celiac disease is the strict elimination of gluten from diets.
\nGenerally, gluten is the term used to describe the alcohol-soluble fraction of storage protein in grain wheat which made up of most diet in western countries [7]. The storage proteins include prolamins (glutenin and gliadins) found in wheat grain, secalin found in rye, hordeins found in barley and avenins found in oats. These storage proteins had been found to contain glutamine and proline residues which are resistant to digestion in the gastrointestinal tract and encourage the deaminization by tissue trans-glutaminase [8]. These proteins when ingested by a genetically susceptible person caused a toxic effect on the gastrointestinal mucosa. The proteins activate the response by cellular immune leading to the injury of the intestinal mucosa which ranges from villous atrophy to infiltration of the lymphocytes. Villous atrophy in human leukocyte antigen (HLA) pre-disposed patient resulted in malabsorption of micro and macronutrients such as fat-soluble vitamins (A, D, E, K), folate, B complex vitamin (Niacin, riboflavin and thiamine), calcium, and iron. To revolve the menace, individuals suffering from a celiac disease needs to strictly adhere to gluten-free diets.
\nGluten-free (GF) diets/foods are defined by the U.S. Food and Drug Administration as a food completely devoid of gluten or does not contain a gluten-containing grain (wheat, barley, oat and rye), flours made from gluten-containing grain in which the gluten had been removed or not removed (wheat flour or starch) and finally, if any of the above-mentioned products contain at least 20 ppm of gluten in food [9]. However, the Commission Regulation of European Union defines a gluten-free diet as a foodstuff that contains a gluten level not exceeding 20 ppm for people who are intolerance to gluten. It was further regulated that food not exceeding 100 ppm in gluten content should be tagged as very low gluten. There is a wide range of palatable and attractive gluten-free diets specifically manufactured for individuals suffering from celiac disease and this include but not limited to GFD baked products, beverage drinks, wines, beers, sourdough etc. [10, 11]. These products are cereal-based food and had gained wide visibility in North and South America, Europe, North Africa and some part of Asia. Gluten-free products’ marketability is estimated to increase in value from US$ 4.18 billion in 2017 to US$ 6.47 billion by 2023 in which gluten-free bread and cookie are estimated to be the most consumed cereal-based GF-food globally [9]. During the production of food products made from gluten, gluten present in the food products is responsible for the elasticity, extensivity and texture resistant if the dough [2, 12]. However, to improve the quality (texture and specific volume) of gluten-free diet/products, hydrocolloids such as hydroxypropylmethylcellulose, xanthan gum, pectin, carboxymethylcellulose are commonly used to improve the baking quality, imparting texture and appearance as well as stability in the gluten-free dough.
\nThough gluten-free products are ideal for consumption by patients living with the celiac disease, it is however low in protein due to the utilization of flour and starches with higher starch to protein content. When flours from pulses are blended with gluten-free cereals, it results in a meal with the complementary amino acid profiles and likewise provides high-quality proteins for bakery purposes. C-ertain species of pseudocereals have been reported to have significant nutritional constituents such as micronutrients, polyphenols, proteins, and dietary fibers when compared with flour produced from cereals [13]. Significant higher mineral content has been reported in gluten-free foods produced from quinoa, millet, oat, amaranth, and buckwheat when compared with those made from rice, maize, and potato starch [13].
\nSome method which had been reported to improve nutritional values and bioavailability of gluten-free bakery goods includes malting and sprouting as these processes help in activating enzymes responsible for the starch, proteins, and lipids breakdown [14, 15]. It has been suggested that gluten-free bakery products should be incorporated with pulses and pseudocereals rather than the use of starches and gluten-free cereals only.
\nA major challenge in the production of gluten-free bakery products is in achieving sensory attributes that are desirable and acceptable by consumers. Gluten-free bakery products are known for their distinct color, texture, appearance, taste, and aroma when compared to those made from wheat flour. Due to complex formulation, gluten-free bakery products tend to appear darker. Regarding wheat products, gluten-free bakery products have lower volumes and harder textures. The acceptability of some gluten-free bakery products has been reported to improve in terms of texture when some proteins were added. In a study by Matos et al. [16], gluten-free muffins were more acceptable by consumers when soy protein isolate was incorporated. In a related study, the acceptability of millet muffins improved in terms of texture when chicken protein isolate and transglutaminase were combined [17]. Future research should focus on how enzymes, proteins, hydrocolloids, and other ingredients can improve the sensory acceptability of gluten-free bakery and pasta products.
\nA very good way of managing celiac disease in immune-mediated patients is the total exclusion of gluten from their diet and diet substitution using gluten-free products. The underlisted products are gluten-free products commonly used in the treatment and management of celiac disease.
\nGF-dough is a thick, malleable mixture of flour (usually cereal - wheat, barley, and rye) and liquid (water) used in the production of bakery products void of gluten. Total removal of gluten from these products enhance safety consumption for celiac disease patients. However, this comes with several difficulties such as poor dough rheological properties, reduced nutritional qualities, off flavor, poor mouth-feel/taste, and more expensive GF-baked product compared with conventional gluten baked products [18, 19, 20].
\nIn research for remedy, food products have been developed from GF-dough made from GF-flour (such as rice, sorghum, buckwheat, amaranth, quinoa, and maize) [19, 21], dairy products [22], dietary fibers [3, 23], and starches [2, 3, 4]. Advantages of these alternatives are low glycemic index, antihypertensive, and antihyperlipidemia [2, 3, 4].
\nRecently, researches have also focused on the production of food products from sourdough rather than from gluten flour [24, 25, 26]. Sourdough is described as a product of a biotechnological process that involves the mixture of flour (cereal) and water, fermented by lactic acid bacteria thereby causing a pleasant sour-tasting dough/product [27]. Sourdough is used to produce several varieties of baked products such as bread, biscuits (crackers) and cakes. Before production, sourdough is characterized by increase dough leavening which promotes GF-end product attractiveness, improved texture and palatability, increase mineral bioavailability, slow down the rate of starch digestion (low glycemic index), antihypertensive potential and extended shelf-life GF-products [19, 26, 28]. Sourdough applications also include the production of novel bioactive compounds which can be used as pre-bioactive starter cultures [28, 29, 30].
\nUnderstanding the functionality of gluten is very important in the baking process of convectional product made from wheat. This gives an insight into the most suitable ingredients that can be considered as gluten replacement. Gluten-free bread has been produced from several types of gluten-free flour such as pseudocereals (e.g., Buckwheat, quinoa, amaranth) [31, 32], cereals (e.g., sorghum, maize, rice) [33, 34], and potato flour [35]. A gluten substitute in bread-making is hydrocolloid. Some commonly reported hydrocolloids include; hydroxypropylmethylcellulose [36]; xanthan gum [32], carboxymethylcellulose, and apple pectic [35]. The application of buckwheat in the production of gluten-free bakery products such as noodle, pasta, cookie, and bread has been reviewed by Giménez-Bastida et al. [37]. The sensory acceptability and present technological limitations of gluten-free pasta and bread were reviewed by Padalino et al. [4]. Strategies for enhancing the quality of gluten-free noodles, pasta, and bread were likewise reviewed by Collar [38], Elgeti et al. [39], and Naqash et al. [40]. Aside from the formulation of gluten-free baked products from cereals and pseudocereals, there had also been a report of the production of GF-baked products such as bread, pastries and cookies from starch isolated from root and tuber crops, banana, cereals and legumes [2, 3, 4, 12, 41].
\nA diet which is free of gluten is the most effective therapy for ailment such as celiac disease. Aside from its beneficial roles in patients with celiac disease, it also has some perceived health benefits such as the regulation weight loss regulation and prevention of gastrointestinal disease. The gluten-free industry was reported to experience a growth of 136% between 2013 and 2015 [42]. Aside from the conventional production of noodles from wheat, noodles are also produced from other uncommon sources such as starches derived from corn, cassava, potatoes, mung beans, and konjac. Grains of rice, oats, and buckwheat are other unconventional sources.
\nSeveral grain varieties were also used in the production of gluten-free noodles with good nutritional and health values. Gluten-free noodles are most suitable for consumption by patients with intolerance to gluten as found in patients with celiac disease. This type of noodles is mostly recommended for anyone who needs to avoid the health challenges posed by the consumption of gluten foods.
\nNoodles made from rice grains are the second most common products after cooked rice grains. Noodles are mostly produced from Indica rice variety and very common in Asia countries like the Philippines, Sri Lanka, Vietnam, Thailand, and Sri Lanka. Fu [43] classified rice noodles into instant, frozen, dried products of shapes and thickness of differing types. With an amylose content of over 22%, Indica rice is most suitable for noodles production. The starch properties determine the structural characteristics of rice noodles as its constituent protein does not play any role in the formation of a stable network structure [44].
\nRice noodles are not prone to breaking apart when pan-fried. They also have an elastic and flexible texture when pan-fried. Majority of consumers preferred rice noodles which are boiled, pan-fried or soup with several ingredients as this noodle products have a smooth taste when eaten and improved eating qualities. Aside from its amylose which is viewed as a possible reason for its suitability in rice noodles production, the exact mechanism is not understood fully.
\nOat grain is a herb plant grown annually. The consumer market for this plant is small. The two major types of oats are Avena nuda L. (naked oats) and Avena sativa L. (Avena sativa). Avena nuda L. is the most commonly cultivated oat in the Gansu, Hebei, Jilin, and Inner Mongolia Provinces in China. Oats are highly nutritious, high-energy and low-sugar food. Oats are usually referred to as healthy foods because of their ability to regulate the metabolism of cholesterol, thereby impeding the onset of certain ailment such as cardiovascular disease, aside its other health benefits [45].
\nBuckwheat flour has protein content within the range of 7–13%, which is significantly higher than the values present in wheat and rice flour. Buckwheat flour is also rich in linoleic and oleic acid with a fat content of about 3%. Rutin, a bioactive compound with hypertensive and hypolipidemic effects, is present in buckwheat flour. Buckwheat noodles are majorly produced in northeast China, Korea, and Japan. Buckwheat noodles processing can be either slit buckwheat noodles or extruded buckwheat noodles. Just like in wheat noodles production, buckwheat noodles are also produced manually or mechanically. In studies by Alamprese et al. [46], pasta product was developed from a combination of eggs, rice flour, and buckwheat flour. This study demonstrates the potential of buckwheat use for noodles production without incorporating wheat flour which is gluten carrying constituent.
\nCassava noodles, potato noodles, konjac noodles, corn noodles, mung bean noodles etc. are some other types of noodles product which are gluten-free. These noodles are rich in nutritional and functional values [47, 48, 49, 50, 51]. Figure 1 shows the flowchart for noodle processing.
\nPotato noodles processing flowchart.
GF-beverage is another GF-product made from GF-cereals such as teff, millet, tigernut, acha, fonio, sorghum among others, consume for prevention/management of celiac disease. Some also play an additional role in the body beyond basic nutritional needs and served as functional drinks. Teff is GF-grain suitable for wheat/barley replacement in production of GF-beverage. Gebremariam et al. [52] reported on Ethiopia local functional drinks made from teff. It was observed that the GF-functional drink exhibits medicinal potential and is suitable for the management of malaria, anemia and diabetes. Badejo et al. [53] developed a GF-beverage from the combination of tigernut and acha varying the blending ratios at 25%. It was observed that the developed beverages contain an appreciable number of phenolic compounds such as gallic acid, rutin, quercetin, ellagic and caffeic acids which may be responsible for higher free radical scavenging abilities reported against DPPH* and ABTS*. Sharma et al. [54] developed prebiotic oligosaccharide rich GF-functional drink from sorghum. They highlighted that the GF-functional drink is suitable for celiac disease patient and contains high calories value, antioxidant capacity, and no changes in sensory properties compared with wheat/barley beverage. GF-beverage are relatively cheap and have extended shelf-life [55].
\nBeer is an alcoholic carbonated, and fermented beverage produced from malted cereal grain (such as wheat, barley, and rye). Consumption of beer is toxic to celiac patients and could results into this autoimmune disorder due to the presence of gliadin from wheat gluten, prolamines/hordeins from barley, and secalins from rye [19, 56]. Scientific research has shown that the successful long-term management of this autoimmune disorder is strict adherence to GF diets [57, 58, 59]. Hence, the needs for GF-beer. European Commission guidelines described GF-beer as pseudo-cereals/cereal malted beer devoid of gluten or beer technologically produced from brewing malt to reduced its gluten content to less than 20 mg/kg [60, 61]. However, controversy exists as US Food and Drug Administration (FDA) proclaim the latter product has the potential to exhibits celiac symptoms in some patients than the former [62, 63].
\nPseudo-cereals malted beer produced from amaranth, buckwheat, and quinoa free of gluten is therefore recommended for celiac patient [56, 57, 64]. These malted beers contain adequate proteins and relatively high starch with sensory attributes slightly lower compared to beer produced from wheat and barley in respect to their taste, aroma, and mouthfeel when adequately mashed, fermented, and stabilized. However, the cost of technology to achieve the aforementioned may inflate the price of pseudo-cereal beer [56, 65].
\nAlternatively, GF-beer can also be produced from GF-cereal such as sorghum, rice, and maize with several brewing conditions been altered such as mashing, sparging, boiling, fermentation temperatures, and pH [66, 67]. This adjustment relatively increases their disparities compared with wheat and barley beer. Comparing GF-sorghum beer with barley beer, the former is rather too viscous, slightly sweetish, and a little bit sour due to the formation of lactic acid [68]. Ceppi and Brenna [69] observed that rice GF-beer were acceptable by consumers but had lower enzymatic activity than barley. Zweytik and Berghofer [68] also reported that GF-maize beer is light yellow with good foam stability, but was relatively poor in taste compared with barley beer. However, they tend to have higher demands by the consumers due to their cheap price [66].
\nOwing to increase in patients suffering from celiac disease as well as gluten intolerance, there had been a rise in consumer demand for gluten-free products as a result of the increase in the number of diagnosis as well as consumers who are making a conscious choice or effort to exclude gluten from their diets. The demand had made gluten-free products one of the fastest-growing market opportunity within the consumer wellness and global health market. For a patient who requires a gluten-free diet, the products must be the same in terms of texture and appearance as conventional gluten-containing products. A market survey of gluten-free food in the United State of America (USA) reveals that the market stood at $2.3 billion in 2019 and it’s estimated to reach $4.5 billion by 2027 according to Gorgitano and Sodano [70]. The United Kingdom (UK) gluten-free products, however, was estimated to be £426 million in 2018 and it’s expected to grow by 40% by 2030. The estimated increase in gluten-free products in the US and UK was due to the facts that gluten-free products are alternative to conventional and traditional grain-based food products such as bakery, pastries, pasta-products which can be made alternatively from other cereals such as maize, sorghum, millet as well as rice [71]. Although the market of gluten-free products had surged higher than the products for other medically diagnosed gluten-related diseases, however, the demand is lower in comparison with gluten-containing products. This had been attributed to the perception of gluten-free products by the consumers as poor or lower quality products with poor appearance, flavor, and texture [1]. However, due to the adherence to gluten-free diets by patients suffering from celiac or gluten intolerance disease, there had been an additional economic burden on the patients due to higher cost price of the products when compared to conventional non-gluten-free products found in the market. In addition to the high selling price of the gluten-free diets, there had been a problem of its availability in the market [72]. A general survey on the market price of gluten-free foods over gluten-containing food products revealed that the price of gluten-free products was 242% more expensive than conventional gluten-containing products. The price was, however, found to be 89% more expensive than its regular products in Chile. The evaluation of the market price, availability and the nutritional composition of gluten-free products by Bagolin do Nascimento et al. [72] at the capital city of Brazil revealed the limitation in the availability of the products in the market coupled with high selling price in comparison with conventional products. Concerning market size among the different segment of gluten-free products, it was reported that gluten-free cookies had more sales and brought in more money compared to gluten-free bread, a reason which could be attributed to the convenience and the quality of the cookie [73]. Other reason could be the importance of gluten in the functional properties of the bread compared to cookie. Gluten gives desirable quality such as the loaf texture and volume to the bread. To make gluten-free foods or products available and avoidable to the patients, the price of the develop GF-foods needs to be considered.
\nAn approximately 1% of the people living in the world today suffers from celiac disease. However, there had been an uprise in the prevalence of the disease due to the underestimation of the disease as it is often left undiagnosed. The only proven remedy to the treatment and management of the disease is the exclusion of wheat or gluten-containing products from their diet and through adherence to gluten-free products/foods. One constrains being perceived by patient suffering from celiac disease is the nutritional imbalance of the diets as a result of the exclusion of gluten and other major gluten-related protein from their diets. Owing to this, it is important that when developing gluten-free diets for patients suffering from celiac disease, the GF-food should be of high nutritional composition, available, and avoidable economically.
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\\n\\n7.8 Governing law: This Publication Agreement and any dispute or claim (including non-contractual disputes or claims) arising out of or in connection with it or its subject matter or formation shall be governed by and construed in accordance with the law of England and Wales. The parties submit to the exclusive jurisdiction of the English courts to settle any dispute or claim arising out of or in connection with this Publication Agreement (including any non-contractual disputes or claims).
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The Corresponding Author (acting on behalf of all Authors) and INTECHOPEN LIMITED, incorporated and registered in England and Wales with company number 11086078 and a registered office at 5 Princes Gate Court, London, United Kingdom, SW7 2QJ conclude the following Agreement regarding the publication of a Book Chapter:
\n\n1. DEFINITIONS
\n\nCorresponding Author: The Author of the Chapter who serves as a Signatory to this Agreement. The Corresponding Author acts on behalf of any other Co-Author.
\n\nCo-Author: All other Authors of the Chapter besides the Corresponding Author.
\n\nIntechOpen: IntechOpen Ltd., the Publisher of the Book.
\n\nBook: The publication as a collection of chapters compiled by IntechOpen including the Chapter. Chapter: The original literary work created by Corresponding Author and any Co-Author that is the subject of this Agreement.
\n\n2. CORRESPONDING AUTHOR'S GRANT OF RIGHTS
\n\n2.1 Subject to the following Article, the Corresponding Author grants and shall ensure that each Co-Author grants, to IntechOpen, during the full term of copyright and any extensions or renewals of that term the following:
\n\nThe aforementioned licenses shall survive the expiry or termination of this Agreement for any reason.
\n\n2.2 The Corresponding Author (on their own behalf and on behalf of any Co-Author) reserves the following rights to the Chapter but agrees not to exercise them in such a way as to adversely affect IntechOpen's ability to utilize the full benefit of this Publication Agreement: (i) reprographic rights worldwide, other than those which subsist in the typographical arrangement of the Chapter as published by IntechOpen; and (ii) public lending rights arising under the Public Lending Right Act 1979, as amended from time to time, and any similar rights arising in any part of the world.
\n\nThe Corresponding Author confirms that they (and any Co-Author) are and will remain a member of any applicable licensing and collecting society and any successor to that body responsible for administering royalties for the reprographic reproduction of copyright works.
\n\nSubject to the license granted above, copyright in the Chapter and all versions of it created during IntechOpen's editing process (including the published version) is retained by the Corresponding Author and any Co-Author.
\n\nSubject to the license granted above, the Corresponding Author and any Co-Author retains patent, trademark and other intellectual property rights to the Chapter.
\n\n2.3 All rights granted to IntechOpen in this Article are assignable, sublicensable or otherwise transferrable to third parties without the Corresponding Author's or any Co-Author’s specific approval.
\n\n2.4 The Corresponding Author (on their own behalf and on behalf of each Co-Author) will not assert any rights under the Copyright, Designs and Patents Act 1988 to object to derogatory treatment of the Chapter as a consequence of IntechOpen's changes to the Chapter arising from translation of it, corrections and edits for house style, removal of problematic material and other reasonable edits.
\n\n3. CORRESPONDING AUTHOR'S DUTIES
\n\n3.1 When distributing or re-publishing the Chapter, the Corresponding Author agrees to credit the Book in which the Chapter has been published as the source of first publication, as well as IntechOpen. The Corresponding Author warrants that each Co-Author will also credit the Book in which the Chapter has been published as the source of first publication, as well as IntechOpen, when they are distributing or re-publishing the Chapter.
\n\n3.2 When submitting the Chapter, the Corresponding Author agrees to:
\n\nThe Corresponding Author will be held responsible for the payment of the Open Access Publishing Fees.
\n\nAll payments shall be due 30 days from the date of the issued invoice. The Corresponding Author or the payer on the Corresponding Author's and Co-Authors' behalf will bear all banking and similar charges incurred.
\n\n3.3 The Corresponding Author shall obtain in writing all consents necessary for the reproduction of any material in which a third-party right exists, including quotations, photographs and illustrations, in all editions of the Chapter worldwide for the full term of the above licenses, and shall provide to IntechOpen upon request the original copies of such consents for inspection (at IntechOpen's option) or photocopies of such consents.
\n\nThe Corresponding Author shall obtain written informed consent for publication from people who might recognize themselves or be identified by others (e.g. from case reports or photographs).
\n\n3.4 The Corresponding Author and any Co-Author shall respect confidentiality rights during and after the termination of this Agreement. The information contained in all correspondence and documents as part of the publishing activity between IntechOpen and the Corresponding Author and any Co-Author are confidential and are intended only for the recipient. The contents may not be disclosed publicly and are not intended for unauthorized use or distribution. Any use, disclosure, copying, or distribution is prohibited and may be unlawful.
\n\n4. CORRESPONDING AUTHOR'S WARRANTY
\n\n4.1 The Corresponding Author represents and warrants that the Chapter does not and will not breach any applicable law or the rights of any third party and, specifically, that the Chapter contains no matter that is defamatory or that infringes any literary or proprietary rights, intellectual property rights, or any rights of privacy. The Corresponding Author warrants and represents that: (i) the Chapter is the original work of themselves and any Co-Author and is not copied wholly or substantially from any other work or material or any other source; (ii) the Chapter has not been formally published in any other peer-reviewed journal or in a book or edited collection, and is not under consideration for any such publication; (iii) they themselves and any Co-Author are qualifying persons under section 154 of the Copyright, Designs and Patents Act 1988; (iv) they themselves and any Co-Author have not assigned and will not during the term of this Publication Agreement purport to assign any of the rights granted to IntechOpen under this Publication Agreement; and (v) the rights granted by this Publication Agreement are free from any security interest, option, mortgage, charge or lien.
\n\nThe Corresponding Author also warrants and represents that: (i) they have the full power to enter into this Publication Agreement on their own behalf and on behalf of each Co-Author; and (ii) they have the necessary rights and/or title in and to the Chapter to grant IntechOpen, on behalf of themselves and any Co-Author, the rights and licenses expressed to be granted in this Publication Agreement. If the Chapter was prepared jointly by the Corresponding Author and any Co-Author, the Corresponding Author warrants and represents that: (i) each Co-Author agrees to the submission, license and publication of the Chapter on the terms of this Publication Agreement; and (ii) they have the authority to enter into this Publication Agreement on behalf of and bind each Co-Author. The Corresponding Author shall: (i) ensure each Co-Author complies with all relevant provisions of this Publication Agreement, including those relating to confidentiality, performance and standards, as if a party to this Publication Agreement; and (ii) remain primarily liable for all acts and/or omissions of each such Co-Author.
\n\nThe Corresponding Author agrees to indemnify and hold IntechOpen harmless against all liabilities, costs, expenses, damages and losses and all reasonable legal costs and expenses suffered or incurred by IntechOpen arising out of or in connection with any breach of the aforementioned representations and warranties. This indemnity shall not cover IntechOpen to the extent that a claim under it results from IntechOpen's negligence or willful misconduct.
\n\n4.2 Nothing in this Publication Agreement shall have the effect of excluding or limiting any liability for death or personal injury caused by negligence or any other liability that cannot be excluded or limited by applicable law.
\n\n5. TERMINATION
\n\n5.1 IntechOpen has a right to terminate this Publication Agreement for quality, program, technical or other reasons with immediate effect, including without limitation (i) if the Corresponding Author or any Co-Author commits a material breach of this Publication Agreement; (ii) if the Corresponding Author or any Co-Author (being an individual) is the subject of a bankruptcy petition, application or order; or (iii) if the Corresponding Author or any Co-Author (being a company) commences negotiations with all or any class of its creditors with a view to rescheduling any of its debts, or makes a proposal for or enters into any compromise or arrangement with any of its creditors.
\n\nIn case of termination, IntechOpen will notify the Corresponding Author, in writing, of the decision.
\n\n6. INTECHOPEN’S DUTIES AND RIGHTS
\n\n6.1 Unless prevented from doing so by events outside its reasonable control, IntechOpen, in its discretion, agrees to publish the Chapter attributing it to the Corresponding Author and any Co-Author.
\n\n6.2 IntechOpen has the right to use the Corresponding Author’s and any Co-Author’s names and likeness in connection with scientific dissemination, retrieval, archiving, web hosting and promotion and marketing of the Chapter and has the right to contact the Corresponding Author and any Co-Author until the Chapter is publicly available on any platform owned and/or operated by IntechOpen.
\n\n6.3 IntechOpen is granted the authority to enforce the rights from this Publication Agreement, on behalf of the Corresponding Author and any Co-Author, against third parties (for example in cases of plagiarism or copyright infringements). In respect of any such infringement or suspected infringement of the copyright in the Chapter, IntechOpen shall have absolute discretion in addressing any such infringement which is likely to affect IntechOpen's rights under this Publication Agreement, including issuing and conducting proceedings against the suspected infringer.
\n\n7. MISCELLANEOUS
\n\n7.1 Further Assurance: The Corresponding Author shall and will ensure that any relevant third party (including any Co-Author) shall, execute and deliver whatever further documents or deeds and perform such acts as IntechOpen reasonably requires from time to time for the purpose of giving IntechOpen the full benefit of the provisions of this Publication Agreement.
\n\n7.2 Third Party Rights: A person who is not a party to this Publication Agreement may not enforce any of its provisions under the Contracts (Rights of Third Parties) Act 1999.
\n\n7.3 Entire Agreement: This Publication Agreement constitutes the entire agreement between the parties in relation to its subject matter. It replaces and extinguishes all prior agreements, draft agreements, arrangements, collateral warranties, collateral contracts, statements, assurances, representations and undertakings of any nature made by or on behalf of the parties, whether oral or written, in relation to that subject matter. Each party acknowledges that in entering into this Publication Agreement it has not relied upon any oral or written statements, collateral or other warranties, assurances, representations or undertakings which were made by or on behalf of the other party in relation to the subject matter of this Publication Agreement at any time before its signature (together "Pre-Contractual Statements"), other than those which are set out in this Publication Agreement. Each party hereby waives all rights and remedies which might otherwise be available to it in relation to such Pre-Contractual Statements. Nothing in this clause shall exclude or restrict the liability of either party arising out of its pre-contract fraudulent misrepresentation or fraudulent concealment.
\n\n7.4 Waiver: No failure or delay by a party to exercise any right or remedy provided under this Publication Agreement or by law shall constitute a waiver of that or any other right or remedy, nor shall it preclude or restrict the further exercise of that or any other right or remedy. No single or partial exercise of such right or remedy shall preclude or restrict the further exercise of that or any other right or remedy.
\n\n7.5 Variation: No variation of this Publication Agreement shall be effective unless it is in writing and signed by the parties (or their duly authorized representatives).
\n\n7.6 Severance: If any provision or part-provision of this Publication Agreement is or becomes invalid, illegal or unenforceable, it shall be deemed modified to the minimum extent necessary to make it valid, legal and enforceable. If such modification is not possible, the relevant provision or part-provision shall be deemed deleted.
\n\nAny modification to or deletion of a provision or part-provision under this clause shall not affect the validity and enforceability of the rest of this Publication Agreement.
\n\n7.7 No partnership: Nothing in this Publication Agreement is intended to, or shall be deemed to, establish or create any partnership or joint venture or the relationship of principal and agent or employer and employee between IntechOpen and the Corresponding Author or any Co-Author, nor authorize any party to make or enter into any commitments for or on behalf of any other party.
\n\n7.8 Governing law: This Publication Agreement and any dispute or claim (including non-contractual disputes or claims) arising out of or in connection with it or its subject matter or formation shall be governed by and construed in accordance with the law of England and Wales. The parties submit to the exclusive jurisdiction of the English courts to settle any dispute or claim arising out of or in connection with this Publication Agreement (including any non-contractual disputes or claims).
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