Four drug delivery systems were formulated by non-covalent functionalization of carboxylated single walled carbon nanotubes using biocompatible polymers as coating agent (i.e., Tween 20, Tween 80, chitosan or polyethylene glycol) for the delivery of levodopa, a drug used in Parkinson's disease. The chemical interaction between the coating agent and carbon nanotubes-levodopa conjugate was confirmed by Fourier transform infrared (FTIR) and Raman studies. The drug release profiles were revealed to be dependent upon the type of applied coating material and this could be further adjusted to a desired rate to meet different biomedical conditions. In vitro drug release experiments measured using UV-Vis spectrometry demonstrated that the coated conjugates yielded a more prolonged and sustained release pattern compared to the uncoated conjugate. Cytotoxicity of the formulated conjugates was studied by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay using normal mouse embryonic fibroblast 3T3 cell line. Compared to the non-coated conjugate, the MTT data indicated that the coating procedure improved the biocompatibility of all systems by 34⁻41% when the concentration used exceeded 100 μg/mL. In conclusion, the comprehensive results of this study suggest that carbon nanotubes-based drug carrier coated with a suitable biomaterial may possibly be a potential nanoparticle system that could facilitate drug delivery to the brain with tunable physicochemical properties.
SnO₂ nanoparticle production using thermal treatment with tin(II) chloride dihydrate and polyvinylpyrrolidone capping agent precursor materials for calcination was investigated. Samples were analyzed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse UV-vis reflectance spectra, photoluminescence (PL) spectra and the electron spin resonance (ESR). XRD analysis found tetragonal crystalline structures in the SnO₂ nanoparticles generated through calcination. EDX and FT-IR spectroscopy phase analysis verified the derivation of the Sn and O in the SnO₂ nanoparticle samples from the precursor materials. An average nanoparticle size of 4–15.5 nm was achieved by increasing calcination temperature from 500 °C to 800 °C, as confirmed through TEM. The valence state and surface composition of the resulting nanoparticle were analyzed using XPS. Diffuse UV-vis reflectance spectra were used to evaluate the optical energy gap using the Kubelka-Munk equation. Greater calcination temperature resulted in the energy band gap falling from 3.90 eV to 3.64 eV. PL spectra indicated a positive relationship between particle size and photoluminescence. Magnetic features were investigated through ESR, which revealed the presence of unpaired electrons. The magnetic field resonance decreases along with an increase of the g-factor value as the calcination temperature increased from 500 °C to 800 °C. Finally, Escherichia coli ATCC 25922 Gram (–ve) and Bacillus subtilis UPMC 1175 Gram (+ve) were used for in vitro evaluation of the tin oxide nanoparticle’s antibacterial activity. This work indicated that the zone of inhibition of 22 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.
Modifications of virus-like nanoparticles (VLNPs) using chemical conjugation techniques have brought the field of virology closer to nanotechnology. The huge surface area to volume ratio of VLNPs permits multiple copies of a targeting ligand and drugs to be attached per nanoparticle. By exploring the chemistry of truncated hepatitis B core antigen (tHBcAg) VLNPs, doxorubicin (DOX) was coupled covalently to the external surface of these nanoparticles via carboxylate groups. About 1600 DOX molecules were conjugated on each tHBcAg VLNP. Then, folic acid (FA) was conjugated to lysine residues of tHBcAg VLNPs to target the nanoparticles to cancer cells over-expressing folic acid receptor (FR). The result demonstrated that the dual bioconjugated tHBcAg VLNPs increased the accumulation and uptake of DOX in the human cervical and colorectal cancer cell lines compared with free DOX, resulting in enhanced cytotoxicity of DOX towards these cells. The fabrication of these dual bioconjugated nanoparticles is simple, and drugs can be easily conjugated with a high coupling efficacy to the VLNPs without any limitation with respect to the cargo's size or charge, as compared with the pH-responsive system based on tHBcAg VLNPs. These dual bioconjugated nanoparticles also have the potential to be modified for other combinatorial drug deliveries.
Herein, a new approach was proposed to produce reduced graphene oxide (rGO) from graphene oxide (GO) using various oil palm wastes: oil palm leaves (OPL), palm kernel shells (PKS) and empty fruit bunches (EFB). The effect of heating temperature on the formation of graphitic carbon and the yield was examined prior to the GO and rGO synthesis. Carbonization of the starting materials was conducted in a furnace under nitrogen gas for 3 h at temperatures ranging from 400 to 900 °C and a constant heating rate of 10 °C/min. The GO was further synthesized from the as-carbonized materials using the 'improved synthesis of graphene oxide' method. Subsequently, the GO was reduced by low-temperature annealing reduction at 300 °C in a furnace under nitrogen gas for 1 h. The IG/ID ratio calculated from the Raman study increases with the increasing of the degree of the graphitization in the order of rGO from oil palm leaves (rGOOPL) < rGO palm kernel shells (rGOPKS) < rGO commercial graphite (rGOCG) < rGO empty fruit bunches (rGOEFB) with the IG/ID values of 1.06, 1.14, 1.16 and 1.20, respectively. The surface area and pore volume analyses of the as-prepared materials were performed using the Brunauer Emmett Teller-Nitrogen (BET-N₂) adsorption-desorption isotherms method. The lower BET surface area of 8 and 15 m2 g-1 observed for rGOCG and rGOOPL, respectively could be due to partial restacking of GO layers and locally-blocked pores. Relatively, this lower BET surface area is inconsequential when compared to rGOPKS and rGOEFB, which have a surface area of 114 and 117 m² g-1, respectively.
The performance of a modified electrode of nanocomposite films consisting of polypyrrole-chitosan-titanium dioxide (Ppy-CS-TiO₂) has been explored for the developing a non-enzymatic glucose biosensors. The synergy effect of TiO₂ nanoparticles (NPs) and conducting polymer on the current responses of the electrode resulted in greater sensitivity. The incorporation of TiO₂ NPs in the nanocomposite films was confirmed by X-ray photoelectron spectroscopy (XPS) spectra. FE-SEM and HR-TEM provided more evidence for the presence of TiO₂ in the Ppy-CS structure. Glucose biosensing properties were determined by amperommetry and cyclic voltammetry (CV). The interfacial properties of nanocomposite electrodes were studied by electrochemical impedance spectroscopy (EIS). The developed biosensors showed good sensitivity over a linear range of 1-14 mM with a detection limit of 614 μM for glucose. The modified electrode with Ppy-CS nanocomposite also exhibited good selectivity and long-term stability with no interference effect. The Ppy-CS-TiO₂ nanocomposites films presented high electron transfer kinetics. This work shows the role of nanomaterials in electrochemical biosensors and describes the process of their homogeneous distribution in composite films by a one-step electrochemical process, where all components are taken in a single solution in the electrochemical cell.
The conventional synthesis route of nanostructured titania-silica (Ti-SiNS) based on sol-gel requires the use of a surfactant-type template that suffers from hazardous risks, environmental concerns, and a tedious stepwise process. Alternatively, biomaterials have been introduced as an indirect template, but still required for pre-suspended scaffold structures, which hinder their practical application. Herein, we report an easy and industrially viable direct-continuous strategy for the preparation of Ti-SiNS from nanostructured-silica (SiNS) using a hydrolyzed rice starch template. This strategy fits into the conventional industrial process flow, as it allows starch to be used directly in time-effective and less complicated steps, with the potential to upscale. The formation of Ti-SiNS is mainly attributed to Ti attachment in the SiNS frameworks after the polycondensation of the sol-gel composition under acidic-media. The SiNS had pseudo-spherical morphology (nanoparticles with the size of 13 to 22 nm), short order crystal structure (amorphous) and high surface area (538.74 m²·g−1). The functionalized SiNS into Ti-SiNS delivered considerable catalytic activity for epoxidation of 1-naphtol into 1,4-naphthoquinone. The described direct-continuous preparation shows great promise for a cheap, green, and efficient synthesis of Ti-SiNS for advanced applications.
An amphotericin B-containing (AmB) solid lipid nanoparticulate drug delivery system intended for oral administration, comprised of bee's wax and theobroma oil as lipid components was formulated with the aim to ascertain the location of AmB within the lipid matrix: (a) a homogenous matrix; (b) a drug-enriched shell; or (c) a drug enriched core. Both the drug-loaded and drug-free nanoparticles were spherical with AmB contributing to an increase in both the z-average diameter (169 ± 1 to 222 ± 2 nm) and zeta potential (40.8 ± 0.9 to 50.3 ± 1.0 mV) of the nanoparticles. A maximum encapsulation efficiency of 21.4% ± 3.0%, corresponding to 10.7 ± 0.4 mg encapsulated AmB within the lipid matrix was observed. Surface analysis and electron microscopic imaging indicated that AmB was dispersed uniformly within the lipid matrix (option (a) above) and, therefore, this is the most suitable of the three models with regard to modeling the propensity for uptake by epithelia and release of AmB in lymph.
The preparation of activated carbon using palm kernel shells as the precursor (PKSAC) was successfully accomplished after the parametric optimization of the carbonization temperature, carbonization holding time, and the ratio of the activator (H₃PO₄) to the precursor. Optimization at 500 °C for 2 h of carbonization with 20% H₃PO₄ resulted in the highest surface area of the activated carbon (C20) of 1169 m² g-1 and, with an average pore size of 27 Å. Subsequently, the preparation of shape-stabilized phase change material (SSPCM-C20) was done by the encapsulation of n-octadecane into the pores of the PKSAC, C20. The field emission scanning electron microscope images and the nitrogen gas adsorption-desorption isotherms show that n-octadecane was successfully encapsulated into the pores of C20. The resulting SSPCM-C20 nano-composite shows good thermal reliability which is chemically and thermally stable and can stand up to 500 melting and freezing cycles. This research work provided a new strategy for the preparation of SSPCM material for thermal energy storage application generated from oil palm waste.
Nanostructured hematite materials for advanced applications are conventionally prepared with the presence of additives, tainting its purity with remnants of copolymer surfactants, active chelating molecules, stabilizing agents, or co-precipitating salts. Thus, preparing nanostructured hematite via additive-free and green synthesis methods remains a huge hurdle. This study presents an environmentally friendly and facile synthesis of spherical nanostructured hematite (Sp-HNP) using rice starch-assisted synthesis. The physicochemical properties of the Sp-HNP were investigated by Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DR UV-Vis), and nitrogen adsorption⁻desorption analysis. The Sp-HNP showed a well-crystallized structure of pure rhombohedral phase, having a spherical-shaped morphology from 24 to 48 nm, and a surface area of 20.04 m²/g. Moreover, the Sp-HNP exhibited enhanced photocatalytic degradation of methylene blue dye, owing to the large surface-to-volume ratio. The current work has provided a sustainable synthesis route to produce spherical nanostructured hematite without the use of any hazardous agents or toxic additives, in agreement with the principles of green chemistry for the degradation of dye contaminant.
The treatment of cancer through chemotherapy is limited by its toxicity to healthy tissues and organs, and its inability to target the cancer site. In this study, we have designed an anticancer nanocomposite delivery system for protocatechuic acid (PCA) using graphene oxide⁻polyethylene glycol as the nanocarrier, and coated with folic acid (GO⁻PEG⁻PCA⁻FA) for targeting the cancer cells. The designed anticancer delivery system was found to show much better anticancer activity than the free drug PCA against liver cancer HEP-G2 cells and human colon cancer HT-29 cells; at same time, it was found to be less toxic to normal fibroblast 3T3 cells. The folate-coated anticancer delivery system was found to show better activity then the free drug and the uncoated anticancer delivery system. The in vitro release of the PCA was found to be sustained in human physiological pHs, i.e., blood pH 7.4 and intracellular lysosomal pH 4.8. These in vitro findings are highly encouraging for further in vivo evaluation studies.
The synergistic effect of using κ-carrageenan bionanocomposites with the hybridization of cellulose nanocrystals (CNCs) and organically modified montmorillonite (OMMT) reinforcements was studied. The effects of different reinforcements and filler contents were evaluated through mechanical testing, and morphological and water uptake properties. The tensile strength and Young's modulus of both bionanocomposites increased with filler loading and optimized at 4%. OMMT incorporation into the κ-carrageenan/CNCs bionanocomposites resulted in further mechanical property improvement with an optimum ratio of 1:1 (CNCs:OMMT) while maintaining high film transparency. X-ray diffraction and morphological analyses revealed that intercalation occurred between the κ-carrageenan bionanocomposite matrix and OMMT. The water uptake of the κ-carrageenan bionanocomposites was significantly reduced by the addition of both CNCs and OMMT. The enhancements in the mechanical properties and performance of the hybrid bionanocomposite indicate compatibility among the reinforcement, biopolymer, and well-dispersed nanoparticles. This renders the hybrid CNC/OMMT/κ-carrageenan nanocomposites extremely promising for food packaging applications.
Herein, we describe the use of gamma irradiation to prepare hydrogels comprising α-cellulose and cellulose nanocrystal (CNC)-reinforced gelatin in the absence of crosslinking agents. In this study, cellulose was extracted from rice husks by an alkali and bleaching treatment followed by acid hydrolysis to produce CNC. A semi-interpenetrating network (semi-IPN) of hydrogels was developed by the miscibility between gelatin and cellulosic materials. Compared to those prepared from α-cellulose, hydrogels prepared by dispersion of CNCs exhibited remarkably enhanced stiffness and swelling properties, which was ascribed to the uniform distribution of CNCs and their increased crystallinity. Improved pore structure, arrangement, and rigidity of CNC-reinforced gelatin hydrogels, which induced the swelling mechanism resulting in higher and faster water uptake was observed with a scanning electron microscope (SEM), compared to cellulose-reinforced gelatin hydrogels. Moreover, in vitro drug profiling demonstrated that CNC/gelatin hydrogels exhibit good drug loading/release behavior and are thus suitable for use in drug-delivery applications.
The combination of compounds with different classes (hydrophobic and hydrophilic characters) in single chitosan carrier is a challenge due to the hydrophilicity of chitosan. Utilization of l-ascorbic acid (LAA) and thymoquinone (TQ) compounds as effective antioxidants is marred by poor bioavailability and uptake. Nanoparticles (NPs) solved the problem by functioning as a carrier for them because they have high surface areas for more efficient delivery and uptake by cells. This research, therefore, synthesized chitosan NPs (CNPs) containing LAA and TQ, CNP-LAA-TQ via ionic gelation routes as the preparation is non-toxic. They were characterized using electron microscopy, zetasizer, UV⁻VIS spectrophotometry, and infrared spectroscopy. The optimum CNP-LAA-TQ size produced was 141.5 ± 7.8 nm, with a polydispersity index (PDI) of 0.207 ± 0.013. The encapsulation efficiency of CNP-LAA-TQ was 22.8 ± 3.2% for LAA and 35.6 ± 3.6% for TQ. Combined hydrophilic LAA and hydrophobic TQ proved that a myriad of highly efficacious compounds with poor systemic uptake could be encapsulated together in NP systems to increase their pharmaceutical efficiency, indirectly contributing to the advancement of medical and pharmaceutical sectors.
Conventional delivery of anticancer drugs is less effective due to pharmacological drawbacks such as lack of aqueous solubility and poor cellular accumulation. This study reports the increased drug loading, therapeutic delivery, and cellular accumulation of silibinin (SLB), a poorly water-soluble phenolic compound using a hydrophobically-modified chitosan nanoparticle (pCNP) system. In this study, chitosan nanoparticles were hydrophobically-modified to confer a palmitoyl group as confirmed by 2,4,6-Trinitrobenzenesulfonic acid (TNBS) assay. Physicochemical features of the nanoparticles were studied using the TNBS assay, and Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) analyses. The FTIR profile and electron microscopy correlated the successful formation of pCNP and pCNP-SLB as nano-sized particles, while Dynamic Light Scattering (DLS) and Field Emission-Scanning Electron Microscopy (FESEM) results exhibited an expansion in size between pCNP and pCNP-SLB to accommodate the drug within its particle core. To evaluate the cytotoxicity of the nanoparticles, a Methylthiazolyldiphenyl-tetrazolium bromide (MTT) cytotoxicity assay was subsequently performed using the A549 lung cancer cell line. Cytotoxicity assays exhibited an enhanced efficacy of SLB when delivered by CNP and pCNP. Interestingly, controlled release delivery of SLB was achieved using the pCNP-SLB system, conferring higher cytotoxic effects and lower IC50 values in 72-h treatments compared to CNP-SLB, which was attributed to the hydrophobic modification of the CNP system.
We have developed gadolinium-based theranostic nanoparticles for co-delivery of drug and magnetic resonance imaging (MRI) contrast agent using Zn/Al-layered double hydroxide as the nanocarrier platform, a naturally occurring phenolic compound, gallic acid (GA) as therapeutic agent, and Gd(NO₃)₃ as diagnostic agent. Gold nanoparticles (AuNPs) were grown on the system to support the contrast for MRI imaging. The nanoparticles were characterized using techniques such as Hi-TEM, XRD, ICP-ES. Kinetic release study of the GA from the nanoparticles showed about 70% of GA was released over a period of 72 h. The in vitro cell viability test for the nanoparticles showed relatively low toxicity to human cell lines (3T3) and improved toxicity on cancerous cell lines (HepG2). A preliminary contrast property test of the nanoparticles, tested on a 3 Tesla MRI machine at various concentrations of GAGZAu and water (as a reference) indicates that the nanoparticles have a promising dual diagnostic and therapeutic features to further develop a better future for clinical remedy for cancer treatment.
pH-sensitive poly(acrylic acid) (PAA) hydrogel reinforced with cellulose nanocrystals (CNC) was prepared. Acrylic acid (AA) was subjected to chemical cross-linking using the cross-linking agent MBA (N,N-methylenebisacrylamide) with CNC entrapped in the PAA matrix. The quantity of CNC was varied between 0, 5, 10, 15, 20, and 25 wt %. X-ray diffraction (XRD) data showed an increase in crystallinity with the addition of CNC, while rheology tests demonstrated a significant increase in the storage modulus of the hydrogel with an increase in CNC content. It was found that the hydrogel reached maximum swelling at pH 7. The potential of the resulting hydrogels to act as drug carriers was then evaluated by means of the drug encapsulation efficiency test using theophylline as a model drug. It was observed that 15% CNC/PAA hydrogel showed the potential to be used as drug carrier system.
Recent biotechnological advances in the food industry have led to the enzymatic production of angiotensin I-converting enzyme (ACE)-inhibitory biopeptides with a strong blood pressure lowering effect from different food proteins. However, the safe oral administration of biopeptides is impeded by their enzymatic degradation due to gastrointestinal digestion. Consequently, nanoparticle (NP)-based delivery systems are used to overcome these gastrointestinal barriers to maintain the improved bioavailability and efficacy of the encapsulated biopeptides. In the present study, the ACE-inhibitory biopeptides were generated from stone fish (Actinopyga lecanora) protein using bromelain and stabilized by their encapsulation in chitosan (chit) nanoparticles (NPs). The nanoparticles were characterized for in vitro physicochemical properties and their antihypertensive effect was then evaluated on spontaneously hypertensive rats (SHRs). The results of a physicochemical characterization showed a small particle size of 162.70 nm, a polydispersity index (pdi) value of 0.28, a zeta potential of 48.78 mV, a high encapsulation efficiency of 75.36%, a high melting temperature of 146.78 °C and an in vitro sustained release of the biopeptides. The results of the in vivo efficacy indicated a dose-dependent blood pressure lowering effect of the biopeptide-loaded nanoparticles that was significantly higher (p < 0.05) compared with the un-encapsulated biopeptides. Moreover, the results of a morphological examination using transmission electron microscopy (TEM) demonstrated the nanoparticles as homogenous and spherical. Thus, the ACE-inhibitory biopeptides stabilized by chitosan nanoparticles can effectively reduce blood pressure for an extended period of time in hypertensive individuals.
Lung cancer, breast cancer and colorectal cancer are the most prevalent fatal types of cancers globally. Gallic acid (3,4,5-trihydroxybenzoic acid) is a bioactive compound found in plants and foods, such as white tea, witch hazel and it has been reported to possess anticancer, antioxidant and anti-inflammatory properties. In this study we have redesigned our previously reported anticancer nanocomposite formulation with improved drug loading based on iron oxide magnetite nanoparticles coated with polyethylene glycol and loaded with anticancer drug gallic acid (Fe₃O₄-PEG-GA). The in vitro release profile and percentage drug loading were found to be better than our previously reported formulation. The anticancer activity of pure gallic acid (GA), empty carrier (Fe₃O₄-PEG) nanocarrier and of anticancer nanocomposite (Fe₃O₄-PEG-GA) were screened against human lung cancer cells (A549), human breast cancer cells (MCF-7), human colon cancer cells (HT-29) and normal fibroblast cells (3T3) after incubation of 24, 48 and 72 h using (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide) MTT assay. The designed formulation (Fe₃O₄-PEG-GA) showed better anticancer activity than free gallic acid (GA). The results of the in vitro studies are highly encouraging to conduct the in vivo studies.
Many people suffer from myopia or hyperopia due to the refractive errors of the cornea all over the world. The use of high refractive index (RI), Abbe number (νd), and visible light transmittance (T%) polymeric contact lenses (CLs) holds great promise in vision error treatment as an alternative solution to the irreversible laser-assisted in situ keratomileusis (LASIK) surgery. Titanium dioxide nanoparticles (TiO2 NPs) have been suggested as a good candidate to rise the RI and maintain high transparency of a poly(methyl methacrylate) (PMMA)-TiO2 nanocomposite. This work includes a preparation of TiO2 NPs using the sol gel method as well as a synthesis of pure PMMA by free radical polarization and PMMA-TiO2 CLs using a cast molding method of 0.005 and 0.01 w/v concentrations and a study of their effect on the aberrated human eye. ZEMAX optical design software was used for eye modeling based on the Liou and Brennan eye model and then the pure and doped CLs were applied. Ocular performance was evaluated by modulation transfer function (MTF), spot diagram, and image simulation. The used criteria show that the best vision correction was obtained by the CL of higher doping content (p < 0.0001) and that the generated spherical and chromatic aberrations in the eye had been reduced.
Graphene (Gr)/gold (Au) and graphene-oxide (GO)/Au nanocomposites (NCPs) were synthesized by performing pulsed-laser-induced photolysis (PLIP) on hydrogen peroxide and chloroauric acid (HAuCl4) that coexisted with Gr or GO in an aqueous solution. A 3-month-long aqueous solution stability was observed in the NCPs synthesized without using surfactants and additional processing. The synthesized NCPs were characterized using absorption spectroscopy, transmission electron microscopy, Raman spectroscopy, energy dispersive spectroscopy, and X-ray diffraction to prove the existence of hybrid Gr/Au or GO/Au NCPs. The synthesized NCPs were further evaluated using the photocatalytic reaction of methylene blue (MB), a synthetic dye, under UV radiation, visible light (central wavelength of 470 nm), and full spectrum of solar light. Both Gr/Au and GO/Au NCPs exhibited photocatalytic degradation of MB under solar light illumination with removal efficiencies of 92.1% and 94.5%, respectively.