ABSTRACT In this study was evaluated the antibacterial activity of textile fibers containing poly (ethylene oxide-b-lactic acid) nanoparticles with incorporated essential oils. The developed system demonstrated antibacterial activity against Staphylococcus aureus, suggesting its potential use as antibacterial agent. Diblock copolymers based on a fixed PEO block (5kDa) and two different PLA segments (4.5 or 10kDa) were used. The morphology, encapsulation efficiency, blending interaction of essential oils (including lavender, tea tree, thyme, cloves, cedar and lemon grass) and polymer and the release kinetics of the active agent in the nanoparticles. The hydrodynamic radius of the nanoparticles determined by light scattering was affected by the size of the poly(lactic acid) block. The in vitro release suggests that the polymeric barrier is able to control the oil release. Antibacterial activity was more effective in textiles with randomly arranged fibers. In agreement with studies from the literature, nanoparticles obtained from copolymers with lower PLA molar mass favored the release of the essential oil mixture. The incorporation process of the essential oils in the textile fibers proved to be efficient, suggesting viability regarding the use of this system in the antibacterial control. The developed systems offer a new strategy for controlled release with antibacterial activity and suggesting a potential application in the footwear industry.
RESUMO Neste estudo foi avaliada a atividade antibacteriana de fibras têxteis contendo nanopartículas de poli(óxido de etileno-b-ácido lático) com óleos essenciais incorporados. O sistema desenvolvido demonstrou atividade antibacteriana contra Staphylococcus aureus, sugerindo seu potencial uso como agente antibacteriano. Foram utilizados copolímeros dibloco baseados em um bloco fixo de PEO (5kDa) e dois segmentos de PLA diferentes (4,5 e 10kDa). A morfologia, a eficiência do encapsulamento, a interação da blenda de óleos essenciais (incluindo, lavanda, melaleuca, tomilho, cravo, cedro e capim limão) e polímero e a cinética de liberação do agente ativo nas nanopartículas foram avaliadas. O raio hidrodinâmico das nanopartículas determinado pela dispersão da luz foi afetado pelo tamanho do bloco de poli(ácido lático). A liberação in vitro sugere que a barreira polimérica é capaz de controlar a liberação de óleo. A atividade antibacteriana foi mais eficaz em tecidos com fibras arranjadas aleatoriamente. De acordo com estudos da literatura, nanopartículas obtidas de copolímeros com menor massa molar de PLA favoreceram a liberação da mistura de óleos essenciais. O processo de incorporação dos óleos essenciais nas fibras têxteis mostrou-se eficiente sugerindo viabilidade quanto ao uso desse sistema no controle antibacteriano. Os sistemas desenvolvidos oferecem uma nova estratégia para a liberação controlada com atividade antibacteriana e apresentam potenciais aplicações na indústria calçadista.
Pluronic® F127 nanoparticles were loaded with citronella essential oil (CEO) and then covered with chitosan-sodium alginate polyelectrolyte complex (PEC). The system was characterized according to size, zeta potential and stability over time. Dynamic light scattering (DLS) in different proportions of water/ethanol as a dispersive medium was important in confirming that PEC covered the F127 nanoparticles. Infrared spectroscopy also indicated interaction of F127 with PEC. The nanoparticle size evaluated by transmission electron microscopy (TEM) and field emission scanning electron microscopy (FESEM) corroborated the value observed in DLS (hydrodynamic radius (RH) range of 100-200 nm). Encapsulation efficiency of 80% for CEO was determined by UV-Vis spectroscopy. The release profile of the CEO was evaluated in phosphate buffer saline (PBS) containing 20% of ethanol and in simulated sweat fluid, achieving 74 and 81%, respectively. The releasing mechanism fitted the Korsmeyer-Peppas mathematical model, indicating Fickian diffusion behavior for both studied media.
Nanoparticles comprised of the poly(ethylene oxide)-b-poly (lactic acid) diblock copolymer (PEO-b-PLA) with and without the incorporation of lavender oil were prepared by nanoprecipitation. Diblock copolymers based on a fixed PEO block (5KDa) and two different PLA segments (4.5 or 10KDa) were used. The morphology, encapsulation efficiency, essential oil-polymer interaction and the release kinetics of the active agent in the nanoparticles, were evaluated. The hydrodynamic radius of the nanoparticles determined by light scattering was affected by the size of the poly(lactic acid) (PLA) block. The lavender essential oil encapsulation efficiency (at a concentration of 0.4 µL mL-1) determined by UV-VIS spectroscopy was in the range of 70-75%. The in vitro release suggests that the polymeric barrier is able to control the oil release.
Abstract This work evaluated the controlled release of cypermethrin pesticide loaded in microspheres of P(3HB)/PCL blends obtained by emulsion-evaporation method. SEM analysis revealed a strong influence of PCL on the porosity of the microspheres. The infrared spectra showed the presence of pesticide in all polymer compositon evaluated. DSC curves showed that with higher content of PCL, decreased the crystallinity degree of polymers, resulting in a faster release of the pesticide. The release assay of cypermethrin suggests that within an interval of four hours the amount of pesticide released varies depending on the composition of the blends.
Resumo A aplicação de polímeros biodegradáveis para encapsular pesticidas é uma estratégia que permite, a partir de diferentes proporções entre os polímeros, modificar o perfil de liberação do agente. Este trabalho avaliou a liberação controlada do pesticida cipermetrina encapsulado em microesferas de blendas de P(3HB)/PCL (100/0, 0/100, 97/03, 95/05, 90/10, 80/20 e 70/30) obtidas pelo método de emulsificação-evaporação do solvente. As imagens de microscopia eletrônica de varredura revelam a forte influência da PCL na porosidade das microesferas. As análises de infravermelho mostraram a presença do pesticida em todas as composições de polímeros avaliadas. O ensaio de liberação de cipermetrina sugere que, no intervalo de 4 horas, o teor de cipermetrina liberada é dependente da composição das blendas utilizadas. As microesferas de PHB e blendas com menores teores de PCL, 97/03 e 95/05 liberaram 75% a 85% enquanto a composição 70/30 liberou 100% de cipermetrina.
<p>In this study, nifedipine (NFP)-loaded polymeric nanocapsules were prepared and characterised with a view to protect the drug from degradation. Nanocapsule suspensions were prepared using two different surfactants (pluronic F68 and polyvinyl alcohol). Physicochemical stability and <italic>in vivo</italic>antihypertensive effect were evaluated. The particle size, zeta potential and entrapment efficiency remained constant during a period of 28 days of exposure under light irradiation. A smaller particle size and a higher zeta potential were obtained for the nanocapsules prepared with Pluronic F68 as surfactant. The solid drug and the nanocapsules were submitted to light exposure for 28 days. After this period of time, the percentage of drug remaining in the PF68NFP and PVANFP nanocapsules was 28.1% and 21.3%, respectively. In contrast, the solid drug was completely degraded after 4 days, suggesting that the nanocapsule suspensions promoted significant protection of the drug against light exposure. In addition, <italic>in vivo</italic> studies were carried out, which demonstrated that the formulations with polyvinyl alcohol exhibited a very rapid onset of action after oral administration in rats and led to faster drug release. The nanoparticles developed can be considered as an alternative for improving NFP stability in liquid formulations.</p>
Soft nanoparticles of size 200-400 nm were obtained from soybean protein isolate (SPI). The particles were formed and suspended in water by the coacervation of aqueous suspensions of SPI in hostile buffered aqueous solutions in the presence of surfactants. We investigate the effect of storage, ionic strength, and concentrations of SPI and surfactant on nanoparticle size and zeta potential. Transmission electron microscopy images and scattering techniques (SLS/ DLS) revealed that the particles are spherical, with hydrophilic chains at the surface.
Biodegradable nanoparticles (NPs) have received considerable attention because of their possible use in the development of strategies for the topical delivery of oils and therapeutic drugs, particularly when drug penetration in dermis is desired. Zein is a prolamine and is a promising material for the design of drug delivery systems. In this study, NPs were prepared with zein and were used to encapsulate and release terpinen-4-ol, which is a therapeutic agent for the treatment of melanoma. The results show that the zein NPs are promising nanostructured systems for the prolonged delivery of T4OL with potential applications in anti-melanoma therapy.
Herein, the emulsifying properties of soy protein isolate (SPI) were highlighted by showing that the macromolecules undergo conformational changes when adsorbed at interfaces. The conformation of protein chains nested at the interfacial region of oil in water (o/w) emulsions by means of X-ray scattering (SAXS) and direct imaging (scanning electron microscopy (SEM)) techniques was investigated. The mean radius of gyration (Rg) for SPI (aq) is 20 nm and increases up to 30 nm in o/w emulsions; the proteins act as amphiphilic molecules by exposing their hydrophobic core to the oil and their hydrophilic amino acid residues to the water phase. By spray drying the emulsions, it was also possible to measure the size (Rg = 40 nm) and to evaluate the morphology of these proteins at the oil/air interface of the respective microcapsules. The walls of microcapsules are fractals of clustered objects with rough surfaces, which are smoothed by the presence of a cross-linking agent.
Neste artigo, as propriedades emulsificantes da proteína isolada de soja (SPI) foram evidenciadas mostrando que estas macromoléculas sofrem mudanças conformacionais quando adsorvidas em interfaces. Investigou-se a conformação das cadeias proteicas ancoradas nas regiões interfaciais de emulsões de óleo em água (o/a) através de técnicas de espalhamento de raios X (SAXS) e de imagem (microscopia eletrônica de varredura (SEM)). O valor médio do raio de giro (Rg) da SPI (aq) é 20 nm e aumenta para 30 nm em emulsões o/a; as proteínas atuam como moléculas anfifílicas expondo seus núcleos hidrofóbicos ao óleo e os resíduos hidrofílicos à fase aquosa. Este valor ainda é maior após o spray drying das emulsões, na interface o/ar das respectivas microcápsulas. As paredes das microcápsulas são fractais de objetos agregados com superfícies rugosas, que são alisadas pela presença de um agente de reticulação.
In this study the viability of using guar gum to form films was investigated along with the effectiveness of the cross-linking process employing 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC) as the cross-linking agent. In addition, the cross-linked films were evaluated considering the water absorption, thermal stability and mechanical properties. The cross-linking process of guar gum films was confirmed by the low solubility in water and through infrared analysis. The results shown that the properties evaluated were affected by the cross-linking process due to changes in the polysaccharide structure. For example, the swelling behavior and water vapor absorption decreased with an increase in the amount of EDC. The EDC content (10-30%) also affected the polymer structure and hydrogen bond formation, reducing the thermal stability of the system.
Films of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) - PHBV with polyethylene glycol (PEG) were prepared by casting solvent evaporation. The thermal behavior, morphology, crystallinity and molecular weight of these films were studied by the following techniques: differential scanning calorimetry (DSC), scanning electron microscopy (SEM), X-ray diffraction (XRD), size exclusion chromatography (SEC). Mixtures of PHBV/PEG showed a high crystallinity degree, measured by XRD, with values ranging between 60 and 90% according to the concentration of PEG. The melting temperature of PHBV decreased with increasing addition of plasticizer (PEG) in the mixture. SEM results showed that the mixtures were uniform, except for the composition 50/50 which proved to be heterogeneous, as evidenced by the presence of two phases. PHBV had molar mass (Mw = 206000 g mol-1), while the introduced PEG molar mass (Mw = 1350 to 1650 g mol-1). The addition of PEG caused the crystallinity of the polymer films to increase owing to the high crystallinity of PEG. The melting point of the PHBV/PEG mixtures also diminished. In addition, SEC analysis of the blends indicated a reduced molar mass for the mixtures in comparison to pure PHBV (100/0).
Drug-loaded films represent an alternative method for the treatment of skin lesions caused by Herpes simplex, since they facilitate delivery of the drug directly at the site of lesion. The objective of this work was to prepare PVA/PAA films containing AC at pH 2.0 and 4.0. The results show that the pH of the film preparations influences the polymer¾drug interaction kinetic order and the degree of swelling. The mechanism of release of AC from the films obtained at pH 4.0 was anomalous, whereas for the films prepared at pH 2.0 the release followed zero-order kinetics.
In this study, drug delivery nanocarriers based on glyceryl tristearate and castor oil at different ratios were prepared by the hot solvent diffusion method. PEG 660-stearate or Poloxamer 188 and soybean lecithin were used as surfactant and co-surfactant, respectively. Structural and physicochemical characteristics of the particles were investigated by means of dynamic light scattering (DLS), differential scanning calorimetry (DSC), wide-angle X-ray scattering (WAXS), atomic force microscopy (AFM) and transmission electron microscopy (TEM and cryo-TEM). DLS data indicated that smaller particles were obtained when the liquid lipid was used alone to prepare nanoemulsions (NEs). TEM and cryo-TEM images showed that NEs presented spherical particles, whereas solid lipid nanoparticles (SLNs) and nanostructured lipid carriers (NLCs) presented more complex shapes. SLNs exhibited lamellar crystal structure, while NLCs displayed a hybrid structure composed of a lamellar crystalline phase in contact with a liquid oil compartment. These experiments contribute to a better understanding of the structure and release performance of these drug carrier systems.
Neste estudo, nanocarreadores lipídicos foram preparados a partir do triestearato de glicerila e óleo de rícino em diferentes proporções pela técnica de difusão do solvente a quente. Estearato de PEG-660 ou Poloxamer 188 e lecitina de soja foram usados como surfactante e cossurfactante, respectivamente. Características estruturais e físico-químicas das partículas foram investigadas por meio de espalhamento de luz dinâmico (DLS), calorimetria exploratória diferencial (DSC), espalhamento de raios X a altos ângulos (WAXS), microscopia de força atômica (AFM) e microscopia eletrônica de transmissão (TEM e cryo-TEM). Aanálise por DLS indicou que partículas menores foram obtidas quando o lipídio líquido foi usado sozinho para obter as nanoemulsões (NEs). Técnicas microscópicas (TEM e cryo-TEM) mostraram que as NEs apresentaram formas esféricas, enquanto as nanopartículas lipídicas sólidas (NLSs) e os carreadores lipídicos nanoestruturados (CLNs) apresentaram formas mais complexas. As NLSs exibiram estrutura cristalina lamelar, enquanto os CLNs exibiram uma estrutura mista composta de fase cristalina lamelar em contato com compartimento oleoso. Estes experimentos contribuem para um melhor entendimento da capacidade de incorporação e liberação de fármacos destes nanocarreadores.
Poly(ethylene-co-methyl acrylate) (EMA) and poly (caprolactone) triol (PCL-T) blends, a biodegradable aliphatic polyester with low molecular weight and moderate water solubility containing diltiazem hydrochloride (DZ) were studied in terms of the thermal and morphological properties, and drug release mechanism. An increase in the PCL-T content in the EMA/PCL-T/DZ films decreased the degree of DZ crystallinity. Drug release from these films is temperature-dependent, and it is possible to modify the drug release rate by adjusting the EMA/PCL-T composition of the blends. The mechanism of drug release is governed by PCL-T melting and PCL-T leaching from EMA matrix.
In plant growth media of low negative charge, potassium (K) is leached out easily with adverse consequences on its availability to plants and on the environment, since all K fertilizers are completely soluble. The objective of this study was to prepare films based on sodium carboxymethylcellulose (CMC), sodium alginate (SA) and a 1:1 (v/v) CMC:SA mixture to incorporate K and investigate its subsequent release. The film properties were evaluated considering miscibility, glass transition temperature, morphology and permeation of potassium. The absence of strong interactions, the small variation in the glass transition temperature and the roughness detected in the cross-section micrographs of the 1:1 CMC:SA mixtures, indicated a partial miscibility among the components. As a consequence of the above-mentioned characteristics, film release of potassium was highest for the 1:1 CMC:SA mixture and lowest for SA. The release mechanism of K from the 1:1 CMC:SA mixture was controlled by a diffusion process, however, associated effects due to swelling and erosion of the matrix films, were observed for the pure CMC and SA systems. Films of CMC, SA and their 1:1 mixture were able to delay the K release, which can bring considerable benefits in terms of plant growth when media with low negative charges are used.
Em meios para crescimento de plantas deficientes em cargas negativas, o potássio (K) é facilmente lixiviado com conseqü ências adversas quanto a sua disponibilidade para as plantas e para o meio ambiente, uma vez que todos os fertilizantes a base de K são completamente solúveis. O objetivo deste estudo foi preparar filmes a partir da carboximetilcelulose de sódio (CMC), alginato de sódio (AS) e da mistura 1:1 (v/v) CMC:AS para incorporação de K e investigar a sua posterior liberação. As propriedades do filmes foram avaliadas considerando a miscibilidade, a temperatura de transição vítrea, morfologia e permeação de potássio. A ausência de interações fortes, a pequena variação na temperatura de transição vítrea e a rugosidade detectada nas micrografias da secção transversal em filmes da mistura CMC:AS (1:1), indicaram miscibilidade parcial entre os componentes. Como conseqü ência das características acima mencionadas, a liberação de potássio foi maior em filmes da mistura CMC:AS (1:1) e menor para a AS. O mecanismo de liberação de K da mistura CMC:AS (1:1) foi controlada por um processo de difusão, no entanto, efeitos associados ao intumescimento e erosão da matriz, foram observados para os sistemas CMC e AS puros. Filmes de CMC, AS e a mistura (1:1) foram capazes de reduzir a velocidade de liberação de K, podendo trazer benefícios consideráveis em termos do crescimento das plantas quando são utilizados meios deficientes em cargas negativas.
This work analyzed the influence from the sequence of mixture for the composite of polypropylene (PP) with 10% by volume of banana fiber (FB) using maleic anhydride grafted polypropylene (PP-MA) as the coupling agent. The thermal, mechanical, water absorption and morphology of the composites were characterized. Three different sequences were used to mix: the processing of all components together (PP + PP-MA + FB), extrusion of PP / PP-MA and after grinding, the mixture was processed with FB ((PP / PP - MA) + FB), and the mixture of PP-MA with FB followed by extrusion of the composite with PP (PP + (PP-MA + FB)). The composites showed higher thermal stability and lower percent crystallinity than the pure PP, regardless of the sequence of mixing. It was found that the mixture of PP + PP-MA + FB processed once had a higher impact resistance. The composites modified with PP-MA, regardless of the sequence of mixture used, showed higher modulus and lower water absorption than the composite without coupling agent. For the tensile strength and modulus of elasticity no significant changes were observed. The images from scanning electron microscopy indicated that FB had higher adhesion for the composites with PP-MA, especially for composition PP + (PP-MA + FB).
Neste trabalho foi analisada a influência da sequência de mistura do compósito de polipropileno (PP) com 10% em volume de fibras de bananeira (FB) utilizando polipropileno enxertado com anidrido maleico (PP-MA) como agente de acoplamento. As propriedades térmicas, mecânicas, absorção de água e morfologia dos compósitos foram caracterizadas. Foram utilizadas 3 sequências de mistura: o processamento de todos os componentes juntos (PP + PP-MA + FB); a extrusão do PP/PP-MA e após moagem, esta mistura foi processada com a FB ((PP + PP-MA) + FB); e a mistura do PP-MA com a FB seguida da extrusão deste compósito com o PP (PP + (PP-MA + FB)). Os compósitos apresentaram maior estabilidade térmica e menor grau de cristalinidade que o PP puro, independentemente da sequência de mistura. Constatou-se que a mistura de PP + PP-MA + FB processada uma única vez apresentou maior resistência ao impacto. Os compósitos modificados com PP-MA, independentemente da sequência de mistura, apresentaram módulo de elasticidade maior e menor absorção de água que o compósito sem agente de acoplamento. Para a resistência à tração máxima e módulo de elasticidade não ocorreram alterações significativas em relação aos métodos de mistura. Na microscopia eletrônica de varredura foi possível observar que as FB apresentaram maior adesão nos compósitos com PP-MA, principalmente para a composição PP + (PP-MA + FB).