Nanostructured Lipid Carriers-Hydrogels System for Drug Delivery: Nanohybrid Technology Perspective.

Advanced hybrid component development in nanotechnology provides superior functionality in the application of scientific knowledge for the drug delivery industry. The purpose of this paper is to review important nanohybrid perspectives in drug delivery between nanostructured lipid carriers (NLC) and hydrogel systems. The hybrid system may result in the enhancement of each component's synergistic properties in the mechanical strength of the hydrogel and concomitantly decrease aggregation of the NLC. The significant progress in nanostructured lipid carriers-hydrogels is reviewed here, with an emphasis on their preparation, potential applications, advantages, and underlying issues associated with these exciting materials.

Carboxymethyl Cellulose Hydrogel from Biomass Waste of Oil Palm Empty Fruit Bunch Using Calcium Chloride as Crosslinking Agent.

Carboxymethyl cellulose (CMC) is modified cellulose extracted from oil palm empty fruit bunch (OPEFB) biomass waste that has been prepared through etherification using sodium monochloroacetate (SMCA) in the presence of sodium hydroxide. In this research, CMC hydrogel was prepared using calcium chloride (CaCl2) as the chemical crosslinker. Throughout the optimization process, four important parameters were studied, which were: (1) CMC concentration, (2) CaCl2 concentration, (3) reaction time, and (4) reaction temperature. From the results, the best gel content obtained was 28.11% at 20% (w/v) of CMC with 1% (w/v) of CaCl2 in 24 h reaction at room temperature. Meanwhile, the degree of swelling for CMC hydrogel was 47.34 g/g. All samples were characterized using FT-IR, XRD, TGA, and FESEM to study and compare modification on the OPEFB cellulose. The FT-IR spectrum of CMC hydrogel showed a shift of COO- peaks at 1585 cm-1 and 1413 cm-1, indicating the substitution of Ca2+ into the CMC molecular chains. The XRD diffractogram of CMC hydrogel showed no observation of sharp peaks, which signified an amorphous hydrogel phase. The CrI value also proved the decrement of the crystalline nature of CMC hydrogel. TGA-DTG thermograms showed that the Tmax of CMC hydrogel at 293.33 °C is slightly better in thermal stability compared to CMC. Meanwhile, the FESEM micrograph of CMC hydrogel showed interconnected pores indicating the crosslinkages in CMC hydrogel. CMC hydrogel was successfully synthesized using CaCl2 as a crosslinking agent, and its swelling ability can be used in various applications such as drug delivery systems, industrial effluent, food additives, heavy metal removal, and many more.

Incorporation of Hydroxyapatite into Glass Ionomer Cement (GIC) Formulated Based on Alumino-Silicate-Fluoride Glass Ceramics from Waste Materials.

Glass ionomer cement (GIC) is a well-known restorative material applied in dentistry. The present work aims to study the effect of hydroxyapatite (HA) addition into GIC based on physical, mechanical and structural properties. The utilization of waste materials namely clam shell (CS) and soda lime silica (SLS) glass as replacements for the respective CaO and SiO2 sources in the fabrication of alumino-silicate-fluoride (ASF) glass ceramics powder. GIC was formulated based on ASF glass ceramics, polyacrylic acid (PAA) and deionized water, while 1 wt.% of HA powder was added to enhance the properties of the cement samples. The cement samples were subjected to four different ageing times before being analyzed. In this study, the addition of HA caused an increment in density and compressive strength results along with ageing time. Besides, X-ray Diffraction (XRD) revealed the formation of fluorohydroxyapatite (FHA) phase in HA-added GIC samples and it was confirmed by Fourier Transform Infrared (FTIR) analysis which detected OH‒F vibration mode. In addition, needle-like and agglomeration of spherical shapes owned by apatite crystals were observed from Field Emission Scanning Electron Microscopy (FESEM). Based on Energy Dispersive X-ray (EDX) analysis, the detection of chemical elements in the cement samples were originated from chemical compounds used in the preparation of glass ceramics powder and also the polyacid utilized in initiating the reaction of GIC.

Preparation and Optimization of Water-Soluble Cationic Sago Starch with a High Degree of Substitution Using Response Surface Methodology.

Modification and characterizations of cationic sago starch with 3-chloro-2-hydroxypropyl trimethylammonium chloride (CHPTAC) prepared via etherification reaction was reported in this study. The optimization of cationic sago starch modification was performed by utilizing the combination of response surface methodology and central composite design (RSM/CCD). The effect of each variable and the interaction between the three variables, the concentration of CHPTAC, concentration of the catalyst NaOH, and the reaction times on the degree of substitution (DS) of the product were investigated and modeled. Moderate conditions were employed and a water-soluble cationic sago starch with high DS value was obtained. Based on RSM, the highest DS = 1.195 was obtained at optimum conditions: 0.615 mol of CHPTAC concentration (CHPTAC/SS = 5), 30% w/v NaOH, and 5 h reaction time, at 60 °C reaction temperature. Furthermore, the cationic sago starch was characterized using Fourier transform infrared spectroscopy, FTIR, X-ray diffraction, XRD, and field emission scanning electron microscopy, FESEM.

Crosslinked Carboxymethyl Sago Starch/Citric Acid Hydrogel for Sorption of Pb2+, Cu2+, Ni2+ and Zn2+ from Aqueous Solution.

In the present study, CMSS (carboxymethyl sago starch)-based hydrogel was synthesized by crosslinking with citric acid via esterification and then applied as a metal sorbent to overcome excessive heavy metal pollution. The CMSS/CA (carboxymethyl sago starch/citric acid) hydrogel was characterized by Fourier Transform Infrared (FT-IR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and X-ray diffraction (XRD). The absorption band at 1726 cm-1 was observed in the FT-IR spectrum of CMSS/CA hydrogel and indicated ester bonds formed. Further findings show that the cross-linkages in the CMSS/CA hydrogel increased the thermal stability of CMSS and various sizes of pores were also shown in the SEM micrograph. Conversely, the removal of heavy metals was analyzed using Inductively Coupled Plasma-Optic Emission Spectra (ICP-OES). The effects of the pH of the metal solution, contact time, initial concentration of the metal ions and temperature on the sorption capacity were investigated. Under optimum condition, the sorption capacity of Pb2+, Cu2+, Ni2+ and Zn2+ onto CMSS/CA hydrogel were 64.48, 36.56, 16.21, 18.45 mg/g, respectively. The experiments demonstrated that CMSS/CA hydrogel has high selectivity towards Pb2+ in both non-competitive and competitive conditions. In conclusion, the CMSS/CA hydrogel as a natural based heavy metal sorption material exhibited a promising performance, especially in the sorption of Pb2+ for wastewater treatment.

Effect of Superheated Steam Treatment on the Mechanical Properties and Dimensional Stability of PALF/PLA Biocomposite.

The effectiveness of superheated steam (SHS) as an alternative, eco-friendly treatment method to modify the surface of pineapple leaf fiber (PALF) for biocomposite applications was investigated. The aim of this treatment was to improve the interfacial adhesion between the fiber and the polymer. The treatment was carried out in an SHS oven for different temperatures (190⁻230 °C) and times (30⁻120 min). Biocomposites fabricated from SHS-treated PALFs and polylactic acid (PLA) at a weight ratio of 30:70 were prepared via melt-blending techniques. The mechanical properties, dimensional stability, scanning electron microscopy (SEM), and X-ray diffraction (XRD) for the biocomposites were evaluated. Results showed that treatment at temperature of 220 °C for 60 min gave the optimum tensile properties compared to other treatment temperatures. The tensile, flexural, and impact properties as well as the dimensional stability of the biocomposites were enhanced by the presence of SHS-treated PALF. The SEM analysis showed improvement in the interfacial adhesion between PLA and SHS-treated PALF. XRD analysis showed an increase in the crystallinity with the addition of SHS-PALF. The results suggest that SHS can be used as an environmentally friendly treatment method for the modification of PALF in biocomposite production.

Gamma-Irradiation Induced Functionalization of Graphene Oxide with Organosilanes.

Gamma-ray radiation was used as a clean and easy method for turning the physicochemical properties of graphene oxide (GO) in this study. Silane functionalized-GO were synthesized by chemically grafting 3-aminopropyltriethoxysilane (APTES) and 3-glycidyloxypropyltrimethoxysilane (GPTES) onto GO surface using gamma-ray irradiation. This established non-contact process is used to create a reductive medium which is deemed simpler, purer and less harmful compared conventional chemical reduction. The resulting functionalized-GO were characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric analysis (TGA), and Raman spectroscopy. The chemical interaction of silane with the GO surface was confirmed by FT-IR. X-ray diffraction reveals the change in the crystalline phases was due to surface functionalization. Surface defects of the GO due to the introduction of silane mioties was revealed by Raman spectroscopy. Thermogravimetric analysis of the functionalized-GO exhibits a multiple peaks in the temperature range of 200-650 °C which corresponds to the degradation of chemically grafted silane on the GO surface.

Preparation, optimization and swelling study of carboxymethyl sago starch (CMSS)-acid hydrogel.

In this study, sago starch was modified in order to enhance its physicochemical properties. Carboxymethylation was used to introduce a carboxymethyl group into a starch compound. The carboxymethyl sago starch (CMSS) was used to prepare smart hydrogel by adding acetic acid into the CMSS powder as the crosslinking agent. The degree of substitution of the CMSS obtained was 0.6410. The optimization was based on the gel content and degree of swelling of the hydrogel. In this research, four parameters were studied in order to optimize the formation of CMSS-acid hydrogel. The parameters were; CMSS concentration, acetic acid concentration, reaction time and reaction temperature. From the data analyzed, 76.69% of optimum gel content was obtained with 33.77 g/g of degree of swelling. Other than that, the swelling properties of CMSS-acid hydrogel in different media such as salt solution, different pH of phosphate buffer saline solution as well as acidic and alkaline solution were also investigated. The results showed that the CMSS-acid hydrogel swelled in both alkaline and salt solution, while in acidic or low pH solution, it tended to shrink and deswell. The production of the hydrogel as a smart material offers a lot of auspicious benefits in the future especially related to swelling behaviour and properties of the hydrogel in different types of media.

Effect of crosslinking concentration on properties of 3-(trimethoxysilyl) propyl methacrylate/N-vinyl pyrrolidone gels.

BACKGROUND: The incorporation of two different monomers, having different properties, in the same polymer molecule leads to the formation of new materials with great scientific and commercial importance. The basic requirements for polymeric materials in some areas of biomedical applications are that they are hydrophilic, having good mechanical and thermal properties, soft, and oxygen-permeable. RESULTS: A series of 3-(trimethoxysilyl) propyl methacrylate/N-vinyl pyrrolidone (TMSPM/NVP) xerogels containing different concentration of ethylene glycol dimethacrylate (EGDMA) as crosslinking agent were prepared by bulk polymerization to high conversion using BPO as initiator. The copolymers were characterized by FTIR. The corresponding hydrogels were obtained by swelling the xerogels in deionized water to equilibrium. Addition of EGDMA increases the transparency of xerogels and hydrogels. The minimum amount of EGDMA required to produce a transparent xerogel is 1%. All the Swelling parameters, including water content (EWC), volume fraction of polymer (ϕ2) and weight loss during swelling decrease with increasing EGDMA. Young's and shear modulus (E and G) increase as EGDMA increases. The hydrogels were characterized in terms of modulus cross-linking density (v e and v t ) and polymer-solvent interaction parameters (χ). Thermal properties include TGA and glass transition temperature (Tg) enhance by adding EGDMA whereas the oxygen permeability (P) of hydrogels decreases as water content decrease. CONCLUSIONS: This study prepared and studied the properties for new copolymer (TMSPM-co-NVP) contains different amounts of (EGDMA). These copolymers possess new properties with potential use in different biomedical applications. The properties of the prepared hydrogels are fit with the standard properties of materials which should be used for contact lenses.

Effect of Maleic Anhydride-Modified Poly(lactic acid) on the Properties of Its Hybrid Fiber Biocomposites.

This work investigated the effect of maleic anhydride (MA)-modified poly(lactic acid) (PLA), which is melt-blended with different untreated and aqueous borax (BR)-treated hybrid oil palm empty fruit bunch fibers (EFBF)/Kenaf core fibers (KCF), and compression-molded into corresponding hybrid biocomposites. These hybrid systems includes BR-treated EFBF/BR-treated KCF reinforced MA-modified PLA i.e., BR(EFBF-KCF)-MAPLA, BR-treated EFBF/BR-treated KCF reinforced unmodified PLA i.e., BR(EFBF-KCF)-PLA, untreated EFBF/untreated KCF reinforced MA-modified PLA i.e., EFBF-KCF-MAPLA, and untreated EFBF/untreated KCF reinforced unmodified PLA i.e., EFBF-KCF-PLA respectively. Characterizations of the hybrid systems revealed that optimal mechanical, physical, morphological, thermal and dynamic mechanical properties were provided by the BR(EFBF-KCF)-MAPLA, resulting from improved interface adhesion, consequent of the synergistic influence of BR treatment of natural fibers, and the compatibilization effect provided by the MA-modified PLA. The grafting degree and efficiency of MA onto the PLA backbone was appreciable, as indicated by direct titration, and through monitoring using Fourier Transform Infrared Spectroscopy (FTIR); thus the MA-modified PLA facilitated the formation of strong interface adhesion with the BR-treated hybrid fibers. The BR(EFBF-KCF)-MAPLA showed promising properties for usage as a bio-inspired, and sustainable alternative fiberboard article.

The usability of ark clam shell (Anadara granosa) as calcium precursor to produce hydroxyapatite nanoparticle via wet chemical precipitate method in various sintering temperature.

This paper reported the uses of ark clam shell calcium precursor in order to form hydroxyapatite (HA) via the wet chemical precipitation method. The main objective of this research is to acquire better understanding regarding the effect of sintering temperature in the fabrication of HA. Throughout experiment, the ratio of Ca:P were constantly controlled, between 1.67 and 2.00. The formation of HA at these ratio was confirmed by means of energy-dispersive X-ray spectroscopy analysis. In addition, the effect of sintering temperature on the formation of HA was observed using X-ray diffraction analysis, while the structural and morphology was determined by means of field emission scanning electron microscopy. The formation of HA nanoparticle was recorded (~35-69 nm) in the form of as-synthesize HA powder. The bonding compound appeared in the formation of HA was carried out using Fourier transform infrared spectroscopy such as biomaterials that are expected to find potential applications in orthopedic and biomedical industries .

Preparation and characterization of irradiated carboxymethyl sago starch-acid hydrogel and its application as metal scavenger in aqueous solution.

Carboxymethyl sago starch-acid hydrogel was prepared via irradiation technique to remove divalent metal ions (Pb, Cu and Cd) from their aqueous solution. The hydrogel was characterized by using Fourier Transform Infrared (FT-IR), scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The removal of these metal ions was analyzed by using inductively coupled plasma-optic emission spectra (ICP-OES) to study the amount of metal uptake by the hydrogel. Parameters of study include effect of pH, amount of sample, contact time, initial concentration of metal solution and reaction temperature. FTIR spectroscopy shows the CMSS hydrogel absorption peaks at 1741cm(-1), 1605cm(-1) and 1430cm(-1) which indicates the substitution of carboxymethyl group of modified sago starch. The degradation temperature of CMSS hydrogel is higher compared to CMSS due to the crosslinking by electron beam radiation and formed a porous hydrogel. From the data obtained, about 93.5%, 88.4% and 85.5% of Pb, Cu and Cd ions has been respectively removed from their solution under optimum condition.

Impact strength and flexural properties enhancement of methacrylate silane treated oil palm mesocarp fiber reinforced biodegradable hybrid composites.

Natural fiber as reinforcement filler in polymer composites is an attractive approach due to being fully biodegradable and cheap. However, incompatibility between hydrophilic natural fiber and hydrophobic polymer matrix restricts the application. The current studies focus on the effects of incorporation of silane treated OPMF into polylactic acid (PLA)/polycaprolactone (PCL)/nanoclay/OPMF hybrid composites. The composites were prepared by melt blending technique and characterize the composites with Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). FTIR spectra indicated that peak shifting occurs when silane treated OPMF was incorporated into hybrid composites. Based on mechanical properties results, incorporation of silane treated OPMF enhances the mechanical properties of unmodified OPMF hybrid composites with the enhancement of flexural and impact strength being 17.60% and 48.43%, respectively, at 10% fiber loading. TGA thermogram shows that incorporation of silane treated OPMF did not show increment in thermal properties of hybrid composites. SEM micrographs revealed that silane treated OPMF hybrid composites show good fiber/matrix adhesion as fiber is still embedded in the matrix and no cavity is present on the surface. Water absorption test shows that addition of less hydrophilic silane treated OPMF successfully reduces the water uptake of hybrid composites.

The influence of green surface modification of oil palm mesocarp fiber by superheated steam on the mechanical properties and dimensional stability of oil palm mesocarp fiber/poly(butylene succinate) biocomposite.

In this paper, superheated steam (SHS) was used as cost effective and green processing technique to modify oil palm mesocarp fiber (OPMF) for biocomposite applications. The purpose of this modification was to promote the adhesion between fiber and thermoplastic. The modification was carried out in a SHS oven at various temperature (200-230 °C) and time (30-120 min) under normal atmospheric pressure. The biocomposites from SHS-treated OPMFs and poly(butylene succinate) (PBS) at a weight ratio of 70:30 were prepared by melt blending technique. The mechanical properties and dimensional stability of the biocomposites were evaluated. This study showed that the SHS treatment increased the roughness of the fiber surface due to the removal of surface impurities and hemicellulose. The tensile, flexural and impact properties, as well as dimensional stability of the biocomposites were markedly enhanced by the presence of SHS-treated OPMF. Scanning electron microscopy analysis showed improvement of interfacial adhesion between PBS and SHS-treated OPMF. This work demonstrated that SHS could be used as an eco-friendly and sustainable processing method for modification of OPMF in biocomposite fabrication.

The effect of fiber bleaching treatment on the properties of poly(lactic acid)/oil palm empty fruit bunch fiber composites.

In this work, biodegradable composites from poly(lactic acid) (PLA) and oil palm empty fruit bunch (OPEFB) fiber were prepared by melt blending method. Prior to mixing, the fiber was modified through bleaching treatment using hydrogen peroxide. Bleached fiber composite showed an improvement in mechanical properties as compared to untreated fiber composite due to the enhanced fiber/matrix interfacial adhesion. Interestingly, fiber bleaching treatment also improved the physical appearance of the composite. The study was extended by blending the composites with commercially available masterbatch colorant.

Preparation and characterization of polyhydroxybutyrate/polycaprolactone nanocomposites.

Polyhydroxybutyrate (PHB)/polycaprolactone (PCL)/stearate Mg-Al layered double hydroxide (LDH) nanocomposites were prepared via solution casting intercalation method. Coprecipitation method was used to prepare the anionic clay Mg-Al LDH from nitrate salt solution. Modification of nitrate anions by stearate anions between the LDH layers via ion exchange reaction. FTIR spectra showed the presence of carboxylic acid (COOH) group which indicates that stearate anions were successfully intercalated into the Mg-Al LDH. The formation of nanocomposites only involves physical interaction as there are no new functional groups or new bonding formed. X-ray diffraction (XRD) and transmission electron microscopy (TEM) indicated that the mixtures of nanocomposites are intercalated and exfoliated types. XRD results showed increasing of basal spacing from 8.66 to 32.97 Å in modified stearate Mg-Al LDH, and TEM results revealed that the stearate Mg-Al LDH layers are homogeneously distributed in the PHB/PCL polymer blends matrix. Enhancement in 300% elongation at break and 66% tensile strength in the presence of 1.0 wt % of the stearate Mg-Al LDH as compare with PHB/PCL blends. Scanning electron microscopy (SEM) proved that clay improves compatibility between polymer matrix and the best ratio 80PHB/20PCL/1stearate Mg-Al LDH surface is well dispersed and stretched before it breaks.

The influence of chemical surface modification of kenaf fiber using hydrogen peroxide on the mechanical properties of biodegradable kenaf fiber/poly(lactic acid) composites.

Bleaching treatment of kenaf fiber was performed in alkaline medium containing hydrogen peroxide solution maintained at pH 11 and 80 °C for 60 min. The bleached kenaf fiber was analyzed using Fourier Transform Infrared (FTIR) and X-ray Diffraction (XRD) analysis. The bleached kenaf fiber was then compounded with poly-(lactic acid) (PLA) via a melt blending method. The mechanical (tensile, flexural and impact) performance of the product was tested. The fiber treatment improved the mechanical properties of PLA/bleached kenaf fiber composites. Scanning electron micrograph (SEM) morphological analysis showed improvement of the interfacial adhesion between the fiber surface and polymer matrix.

Synthesis, characterization, and antimicrobial properties of copper nanoparticles.

Copper nanoparticle synthesis has been gaining attention due to its availability. However, factors such as agglomeration and rapid oxidation have made it a difficult research area. In the present work, pure copper nanoparticles were prepared in the presence of a chitosan stabilizer through chemical means. The purity of the nanoparticles was authenticated using different characterization techniques, including ultraviolet visible spectroscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The antibacterial as well as antifungal activity of the nanoparticles were investigated using several microorganisms of interest, including methicillin-resistant Staphylococcus aureus, Bacillus subtilis, Pseudomonas aeruginosa, Salmonella choleraesuis, and Candida albicans. The effect of a chitosan medium on growth of the microorganism was studied, and this was found to influence growth rate. The size of the copper nanoparticles obtained was in the range of 2-350 nm, depending on the concentration of the chitosan stabilizer.

Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

Mechanical, thermal and morphological properties of poly(lactic acid)/epoxidized palm olein blend.

Poly(lactic acid) (PLA) is known to be a useful material in substituting the conventional petroleum-based polymer used in packaging, due to its biodegradability and high mechanical strength. Despite the excellent properties of PLA, low flexibility has limited the application of this material. Thus, epoxidized palm olein (EPO) was incorporated into PLA at different loadings (1, 2, 3, 4 and 5 wt%) through the melt blending technique and the product was characterized. The addition of EPO resulted in a decrease in glass transition temperature and an increase of elongation-at-break, which indicates an increase in the PLA chain mobility. PLA/EPO blends also exhibited higher thermal stability than neat PLA. Further, the PLA/1 wt% EPO blend showed enhancement in the tensile, flexural and impact properties. This is due to improved interaction in the blend producing good compatible morphologies, which can be revealed by Scanning Electron Microscopy (SEM) analysis. Therefore, PLA can be efficiently plasticized by EPO and the feasibility of its use as flexible film for food packaging should be considered.