Francisco Rodríguez-Félix

Micro- and Nanoparticles by Electrospray: Advances and Applications in Foods

Micro- and nanotechnology are tools being used strongly in the area of food technology. The electrospray technique is booming because of its importance in developing micro- and nanoparticles containing an active ingredient as bioactive compounds, enhancing molecules of flavors, odors, and packaging coatings, and developing polymers that are obtained from food (proteins, carbohydrates), as chitosan, alginate, gelatin, agar, starch, or gluten. The electrospray technique compared to conventional techniques such as nanoprecipitation, emulsion-diffusion, double-emulsification, and layer by layer provides greater advantages to develop micro- and nanoparticles because it is simple, low cost, uses a low amount of solvents, and products are obtained in one step. This technique could also be applied in the agrifood sector for the preparation of controlled and/or prolonged release systems of fertilizer or agrochemicals, for which more research must be conducted.

Preparation of extruded polyethylene/chitosan blends compatibilized with polyethylene-graft-maleic anhydride

Novel films of polyethylene and chitosan were obtained using extrusion. These polymers have interesting properties, and processing them with methods that are of high use in the industry, such as the extrusion method, can have a significant effect on the potential applications of these materials. The individual materials were thermally characterized; after this, extruded films of low density polyethylene and chitosan mixtures were prepared with the addition of polyethylene-graft-maleic anhydride as a compatibilizer for the blends, and glycerol, as a plasticizer for chitosan. The use of compatibilizer and plasticizer agents improved the processability and compatibility of the mixtures, as well as their mechanical properties, as revealed by mechanical property measurements and scanning electron microscopy. It was possible to prepare blends with a maximum chitosan content of 20 wt%. The material stiffness increased with the increase of chitosan in the sample. FTIR studies revealed the existence of an interaction between the compatibilizer and chitosan.

Extruded films of blended chitosan, low density polyethylene and ethylene acrylic acid

The obtaining of chitosan extruded films was possible by using low density polyethylene (LDPE) as a matrix polymer and ethylene-acrylic acid copolymer as an adhesive, in order to ensure adhesion in the interphase of the immiscible polymers. The obtained blend films were resistant; however, a reduction in the mechanical resistance was observed as chitosan concentration increased. The thermal stability of the films showed a certain grade of interaction between polymers as seen in FTIR spectra. The antifungal activity of the extruded films was assessed against Aspergillus niger and high inhibition percentages were observed, which may be mainly attributed to barrier properties of the extruded films and the limited oxygen availability, resulting in the inability of the fungi to grow. A low adherence of fungal spores to the material surface was observed, mainly in areas with chitosan clumps, which can serve as starting points for material degradation.

Functionalization of chitosan by a free radical reaction: Characterization, antioxidant and antibacterial potential

Chitosan was functionalized with epigallocatechin gallate (EGCG) by a free radical-induced grafting procedure, which was carried out by a redox pair (ascorbic acid/hydrogen peroxide) as the radical initiator. The successful preparation of EGCG grafted-chitosan was verified by spectroscopic (UV, FTIR and XPS) and thermal (DSC and TGA) analyses. The degree of grafting of phenolic compounds onto the chitosan was determined by the Folin-Ciocalteu procedure. Additionally, the biological activities (antioxidant and antibacterial) of pure EGCG, blank chitosan and EGCG grafted-chitosan were evaluated. The spectroscopic and thermal results indicate chitosan functionalization with EGCG; the EGCG content was 25.8mg/g of EGCG grafted-chitosan. The antibacterial activity of the EGCG grafted-chitosan was increased compared to pure EGCG or blank chitosan against S. aureus and Pseudomonas sp. (p<0.05). Additionally, EGCG grafted-chitosan showed higher antioxidant activity than blank chitosan. These results indicate that EGCG grafted-chitosan might be useful in active food packaging.

Preparation and characterization of durum wheat (Triticum durum) straw cellulose nanofibers by electrospinning.

Cellulose nanofibers from durum wheat straw ( Triticum durum ) were produced and characterized to study their potential as reinforcement fibers in biocomposites. Cellulose was isolated from wheat straw by chemical treatment. Nanofibers were produced via an electrospinning method using trifluoroacetic acid (TFA) as the solvent. The nanofibers were 270 ± 97 nm in diameter. Analysis of the FT-IR spectra demonstrated that the chemical treatment of the wheat straw removed hemicellulose and lignin. XRD revealed that the crystallinity of the cellulose was reduced after electrospinning, but nanofibers remained highly crystalline. The glass transition temperature (T(g) value) of the fibers was 130 °C, higher than that of cellulose (122 °C), and the degradation temperature of the fibers was 236 °C. Residual TFA was not present in the nanofibers as assessed by the FT-IR technique.

Preparation, Characterization and Release of Urea from Wheat Gluten Electrospun Membranes

Homogeneous and thin porous membranes composed of oriented fibers were obtained from wheat gluten (WG) using the electrospinning technique. SEM micrographs showed an asymmetric structure and some porosity, which, in addition to a small thickness of 40 μm, are desirable characteristics for the membranes’ potential application in release systems. The membranes were loaded with urea to obtain pastilles. FT-IR and DSC studies confirmed the existence of interactions via hydrogen bonding between urea and WG proteins. The pastilles were studied as prolonged-released systems of urea in water. The release of urea during the first 10 min was very fast; then, the rate of release decreased as it reached equilibrium at 300 min, with a total of ≈98% urea released. TGA analysis showed that the release system obtained is thermally stable up to a temperature of 117 °C. It was concluded that a prolonged-release system of urea could be satisfactorily produced using WG fibers obtained by electrospinning for potential application in agricultural crops.

Physicochemical and Antioxidant Properties of Chitosan Films Incorporated with Cinnamon Oil

Chitosan films (CF) with cinnamon bark oil (CO) incorporated at 0% (control), 0.25%, 0.5%, and 1.0% v/v were prepared by an emulsion method. The films were characterized based on their physical properties (solubility, water vapor permeability, optical property, and microstructure) and antioxidant properties (DPPH, ABTS, and its protective effects on human erythrocytes). The results showed that the incorporation of 0.5 and 1.0% of CO into the CF significantly decreased its solubility to 22% of the control (). The water vapor permeability of the CF-CO was significantly reduced to 40% with low concentrations of CO (0.25%) incorporated into the CF. In general, the films presented a yellow coloration and an increase in transparency with the incorporation of CO into the CF. It was also observed that the incorporation of CO increased the antioxidant activity between 6.0-fold and 14.5-fold compared to the control, and the protective capacity against erythrocyte hemolysis increased by as much as 80%.

Preparation and Characterization of Films Extruded of Polyethylene/Chitosan Modified with Poly(lactic acid)

The use of mixtures of synthetic and natural polymers is a potential option to reduce the pollution by plastic waste. In this work, the method for the chemical modification of chitosan with poly(lactic acid) was developed; then, the preparation of films of blends of polyethylene and chitosan-poly(lactic acid) produced by an extrusion method using polyethylene-graft maleic anhydride as a compatibilizer. It was possible to obtain films with a maximum content of 20 wt% and 30 wt%, chitosan, with and without compatibilizer, respectively. Scanning electron microscope (SEM) analysis showed a homogeneous surface on all films. The addition of the compatibilizer had a significant effect on the mechanical properties of the films, such as an increase in Young’s modulus and a decrease in the elongation at break; additionally, the compatibilizer promotes thermal degradation in a single step and gives the film a slight increase in thermal resistance. These results are attributed to an improved interaction in the interface of polyethylene and chitosan-poly(lactic acid), promoted by the compatibilizer.

Preparation and characterization of films made of poly(l-lactic acid)/poly(l-lactic acid) grafted maleic anhydride/epigallocatechin gallate blends for antibacterial food packaging

The antimicrobial activity of films made of poly(l-lactic acid)/poly(l-lactic acid) grafted maleic anhydride(copolymer)/epigallocatechin gallate(EGCG) blend was determined. The effect of epigallocatechin gallate incorporation (0.03, 0.5, 5, and 10 wt%) as a natural antibacterial was determined by direct contact, solid and liquid culture media. The film antimicrobial activity was evaluated against two bacteria (gram-negative: Pseudomonas spp.; gram-positive: Staphylococcus aureus). The copolymer was prepared and characterized by Fourier transform infrared analysis and Molau test. Furthermore, the degree of grafting was determined. The epigallocatechin gallate migration profile through the films were determined and the minimum epigallocatechin gallate concentration in films required to show antibacterial activity was evaluated. The results showed that only the films with 10 wt% epigallocatechin gallate significantly affected (p < 0.05) the cell morphology and inhibited the growth of S. aureus (56% with copolymer and 55% inhibition without copolymer) and Pseudomonas spp. (28% inhibition, with and without copolymer). Incorporating copolymer inhibited the growth of Pseudomonas spp. and induced morphological changes in S. aureus. The diffusion coefficient was dependent on the presence of copolymer, which increased the epigallocatechin gallate release rate. Incorporating epigallocatechin gallate and copolymer modified the film properties. Fourier transform infrared analysis indicated hydrogen bonds which were attributed to the interaction between copolymer and epigallocatechin gallate. The results demonstrate the potential application of poly(l-lactic acid) (biodegradable polymer) and copolymers in active packaging, as well as the importance of incorporating epigallocatechin gallate as a natural antibacterial agent.

Engineering and antibacterial properties of low-density polyethylene films with incorporated epigallocatechin gallate

The antibacterial activity of low-density polyethylene/adhesive resin (10%)/epigallocatechin gallate (0.03, 0.5, 5, and 10%) extrusion cast films were evaluated against Staphylococcus aureus (gram positive) and Pseudomonas sp. (gram negative) via direct contact and in solid and liquid culture media. The epigallocatechin gallate concentration in the active films was established per the in vitro antibacterial analysis of pure epigallocatechin gallate against S. aureus and Pseudomonas sp. The epigallocatechin gallate migration profile and concentration required to inhibit bacterial growth in broth were determined. In addition, the effects of epigallocatechin gallate and adhesive resin on the mechanical, color, and thermal film properties were investigated. The results indicate that pure epigallocatechin gallate inhibited the growth of both bacteria. However, only the films with 10 wt% epigallocatechin gallate (with and without adhesive resin) induced morphological changes and inhibited the growth of S. aureus (p < 0.05). In addition, the films with 10 wt% epigallocatechin gallate (with adhesive resin) induced morphological changes in Pseudomonas sp. (p < 0.05). The adhesive resin increased the epigallocatechin gallate release rate in the migration profile (p < 0.05). The epigallocatechin gallate and adhesive resin modified the film properties (p < 0.05). Fourier transform infrared analysis indicated hydrogen bonds between the adhesive resin and epigallocatechin gallate. This study demonstrated that epigallocatechin gallate is a potential antibacterial agent and that adhesive resin provides advantages to active films.