The occurrence and fate of antibiotic compounds in water can adversely affect human and animal health; hence, the removal of such substrates from soil and water is indispensable. Herein, we described the synthesis method of mesoporous carbon (MPC) via the pyrolysis route from a coordination polymer Fe-based MIL-53 (or MIL-53, shortly). The MPC structure was analyzed by several physical techniques such as SEM, TEM, BET, FT-IR, VSM, and XRD. The response surface methodology (RSM) was applied to find out the effects of initial concentration, MPC dosage, and pH on the removal efficiency of trimethoprim (TMP) and sulfamethoxazole (SMX) antibiotics in water. Under the optimized conditions, the removal efficiencies of TMP and SMX were found to be 87% and 99%, respectively. Moreover, the adsorption kinetic and isotherm studies showed that chemisorption and the monolayer adsorption controlled the adsorption process. The leaching test and recyclability studies indicated that the MPC structure was stable and can be reused for at least four times without any considerable change in the removal efficiency. Plausible adsorption mechanisms were also addressed in this study. Because of high maximum adsorption capacity (85.5 mg/g and 131.6 mg/g for TMP and SMX, respectively) and efficient reusability, MPC is recommended to be a potential adsorbent for TMP and SMX from water media.
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.
We have synthesized a graphene oxide (GO)-based theranostic nanodelivery system (GOTS) for magnetic resonance imaging (MRI) using naturally occurring protocatechuic acid (PA) as an anticancer agent and gadolinium (III) nitrate hexahydrate (Gd) as the starting material for a contrast agent,. Gold nanoparticles (AuNPs) were subsequently used as second diagnostic agent. The GO nanosheets were first prepared from graphite via the improved Hummer's protocol. The conjugation of the GO and the PA was done via hydrogen bonding and π-π stacking interactions, followed by surface adsorption of the AuNPs through electrostatic interactions. GAGPA is the name given to the nanocomposite obtained from Gd and PA conjugation. However, after coating with AuNPs, the name was modified to GAGPAu. The physicochemical properties of the GAGPA and GAGPAu nanohybrids were studied using various characterization techniques. The results from the analyses confirmed the formation of the GOTS. The powder X-ray diffraction (PXRD) results showed the diffractive patterns for pure GO nanolayers, which changed after subsequent conjugation of the Gd and PA. The AuNPs patterns were also recorded after surface adsorption. Cytotoxicity and magnetic resonance imaging (MRI) contrast tests were also carried out on the developed GOTS. The GAGPAu was significantly cytotoxic to the human liver hepatocellular carcinoma cell line (HepG2) but nontoxic to the standard fibroblast cell line (3T3). The GAGPAu also appeared to possess higher T1 contrast compared to the pure Gd and water reference. The GOTS has good prospects of serving as future theranostic platform for cancer chemotherapy and diagnosis.
Starch blend films made from sago and mung bean were prepared by casting with glycerol as the plasticizer and subsequently exposed to ultraviolet (UV) irradiation for 2 h. The films were characterized by thickness, moisture sorption isotherms, X-ray diffraction and Fourier transform infrared (FTIR) spectroscopy. All films produced were colorless while incorporation of glycerol resulted in more flexible and manageable films. Moisture sorption isotherms for all films showed sigmoidal shape and the control films showed slightly higher curve than treated films. While for X-ray analysis, the control and treated films for all formulations showed similar pattern, however for treated films showed more crystalline character. UV radiation showed affect on X-ray diffraction and sorption isotherms; however the UV radiation did not affect the spectra pattern of FTIR.
A novel method of preparing reduced graphene oxide (RGOX) from graphene oxide (GOX) was developed employing vegetable extract, Chenopodium album, as a reducing and stabilizing agent. Chenopodium album is a green leafy vegetable with a low shelf life, fresh leaves of this vegetable are encouraged to be used due to high water content. The previously modified 'Hummers method' has been in practice for the preparation of GOX by using precursor graphite powder. In this study, green synthesis of RGOX was functionally verified by employing FTIR and UV-visible spectroscopy, along with SEM and TEM. Our results demonstrated typical morphology of RGOX stacked in layers that appeared as silky, transparent, and rippled. The antibacterial activity was shown by analyzing minimal inhibitory concentration values, agar diffusion assay, fluorescence techniques. It showed enhanced antibacterial activity against Gram-positive and Gram-negative bacteria in comparison to GOX. It has also been shown that the synthesized compound exhibited enhanced antibiofilm activity as compared to its parent compound. The efficacy of RGOX and GOX has been demonstrated on a human breast cancer cell line, which suggested RGOX as a potential anticancer agent.
This study reports the application of hydrated lime for the effective adsorption of the heavy mercury metal from the aqueous phase solutions. Initially, hydrated lime was subjected to structural characterization and thermal stability analysis. The FT-IR spectrum analysis revealed that the existence of the O-H bonds as a confirmation of hydrated lime formation. Subsequently, the XRD powder-based analysis demonstrated that most of the hydrated lime is pure crystalline material known as Portlandite while a small amount of calcite is also present in the structure of the hydrated lime. The thermal stability analysis revealed that the hydrated lime is highly thermally stable under harsh conditions without decomposing at higher temperatures up to 500 °C. Furthermore, the hydrated lime was subjected to the selective adsorption of heavy metal mercury to investigate the potential influence of the adsorbent particle size and loading on adsorption capacity. The results demonstrated that the decrease in the adsorbent particle size leads to the improvement in the mercury adsorption attributing to the rise in specific surface area. The enhancement in the loading of the adsorbent resulted in a reduction in mercury adsorption directing to the fact that already adsorbed metal ions onto the adsorbent surface lead to hindrance for the adsorption of other ions of heavy metal. These results lead to a significant impact on modern in inventing different adsorbents with promising water treatment efficiency for more industrial applications and the related recovery of mercury.
The various composition multicomponent chitosan/fish collagen/glycerin 3D porous scaffolds were developed and investigated the effect of various composition chitosan/fish collagen/glycerin on scaffolds morphology, mechanical strength, biostability and cytocompatibility. The scaffolds were fabricated via freeze-drying technique. The effects of various compositions consisting in 3D scaffolds were investigated via FT-IR analysis, porosity, swelling and mechanical tests, and effect on the morphology of scaffolds investigated microscopically. The biostability and cytocompatibility tests were used to explore the ability of scaffolds to use for tissue engineering application. The average pore sizes of scaffolds were in range of 100.73±27.62-116.01±52.06, porosity 71.72±3.46-91.17±2.42%, tensile modulus in dry environment 1.47±0.08-0.17±0.03MPa, tensile modulus in wet environment 0.32±0.03-0.14±0.04MPa and biodegradation rate (at day 30) 60.38±0.70-83.48±0.28%. In vitro culture of human fibroblasts and keratinocytes showed that the various composition multicomponent 3D scaffolds were good cytocompatibility however, the scaffolds contained high amount of fish collagen excellently facilitated cell proliferation and adhesion. It was found that the high amount fish collagen and glycerin scaffolds have high porosity, enough mechanical strength and biostability, and excellent cytocompatibility.
New acrylic microspheres were synthesised by photopolymerisation where the succinimide functional group was incorporated during the microsphere preparation. An optical biosensor for urea based on reflectance transduction with a large linear response range to urea was successfully developed using this material. The biosensor utilized succinimide-modified acrylic microspheres immobilized with a Nile blue chromoionophore (ETH 5294) for optical detection and urease enzyme was immobilized on the surface of the microspheres via the succinimide groups. No leaching of the enzyme or chromoionophore was observed. Hydrolysis of the urea by urease changes the pH and leads to a color change of the immobilized chromoionophore. When the color change was monitored by reflectance spectrophotometry, the linear response range of the biosensor to urea was from 0.01 to 1,000 mM (R2 = 0.97) with a limit of detection of 9.97 μM. The biosensor response showed good reproducibility (relative standard deviation = 1.43%, n = 5) with no interference by major cations such as Na+, K+, NH4+ and Mg2+. The use of reflectance as a transduction method led to a large linear response range that is better than that of many urea biosensors based on other optical transduction methods.
Buffing dust, generated from tannery industries, is a source of air pollution in Pakistan. Valorization of the waste into another useful material is important to deal with the environmental pollution, while reducing waste disposal costs in landfills. To demonstrate its technological strength, this work fabricates a thermal insulation material made of plaster of Paris and the buffing dust (from tanning waste) in the form of a composite with superior mechanical properties and low thermal conductivity. Buffing dust with concentrations ranging from 5 to 20% (w/w) were loaded in the composite. The samples synthesized were made slurry of plaster of Paris, buffing dust, and water at ambient temperature. The physico-mechanical properties of composite were analyzed. It was found that the composite had better thermal insulation properties than the panels of the plaster of Paris. Its thermal conductivity was reduced to 15% after adding buffing dust (20% w/w). All the materials had physico-chemical properties like tensile strength (0.02 MPa and 0.06 MPa), density (700-400 kg/m3), water absorption (5.2-8.6%) and thermal conductivity (0.17000-0.09218 W/m-K). Thermogravimetric analysis showed that the material was thermally stable at temperatures ranging from 145 to 177 °C, while FT-IR results revealed that the composite contained O-H, N-H, and CO functional groups. SEM analysis displayed that the composite's homogeneity was reduced with low voids due to buffing dust addition, while EDX analysis showed that the composite contained 23.62% of S, 26.76% of Ca, 49.2% of O and 0.42% of C. This implies that buffing dust could be recycled to manufacture heat insulation materials for construction sector to reduce air pollution, while minimizing energy consumption. By integrating the buffing dust from tanning waste and the plaster of Paris as a composite for construction sector, this work promotes the recycling of unused waste, while saving public funds. Instead of paying landfill fees and polluting soil, the waste may be recycled at lower cost, while reducing environmental damage.
A chemical method to synthesize amorphous silica nanoparticles from the incinerated paddy straw has been introduced. The synthesis was conducted through the hydrolysis by alkaline-acidic treatments. As a result, silica particles produced with the sizes were ranging at 60-90 nm, determined by high-resolution microscopy. The crystallinity was confirmed by surface area electron diffraction. Apart from that, chemical and diffraction analyses for both rice straw ash and synthesized silica nanoparticles were conducted by X-ray diffraction and Fourier-transform infrared spectroscopy. The percentage of silica from the incinerated straw was calculated to be 28.3. The prominent surface chemical bonding on the generated silica nanoparticles was with Si-O-Si, stretch of Si-O and symmetric Si-O bonds at peaks of 1090, 471, and 780 cm-1, respectively. To confirm the impurities of the elements in the produced silica, were analyzed using X-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. The stability of silica nanoparticles was investigated using thermogravimetric analysis and zeta potential. The measured size from zeta potential analysis was 411.3-493 nm and the stability of mass reduction was located at 200 °C with final amount of mass reduced ∼88% and an average polydispersity Index was 0.195-0.224.
Tissue engineering scaffolds with oxygen generating elements have shown to be able to increase the level of oxygen and cell survivability in specific conditions. In this study, biphasic calcium phosphate (BCP) scaffolds with the composition of 60% hydroxyapatite (HA) and 40% beta-tricalcium phosphate (β-TCP), which have shown a great potential for bone tissue engineering applications, were fabricated by a direct-write assembly (robocasting) technique. Then, the three-dimensional (3D)-printed scaffolds were coated with different ratios of an oxygen releasing agent, calcium peroxide (CPO), which encapsulated within a polycaprolactone (PCL) matrix through dip-coating, and used for in situ production of oxygen in the implanted sites. The structure, composition and morphology of the prepared scaffolds were characterized by different techniques. The oxygen release kinetics and biological investigations of the scaffolds were also studied in vitro. The results showed that oxygen release behaviour was sustained and dependant on the concentration of CPO encapsulated in the PCL coating matrix. It was also demonstrated that the coated scaffolds, having 3% CPO in the coating system, could provide a great potential for promoting bone ingrowth with improving osteoblast cells viability and proliferation under hypoxic conditions. The findings indicated that the prepared scaffolds could play a significant role in engineering of large bone tissue implants with limitations in oxygen diffusion.
In order to improve the membrane lipophilicity and the affinity towards the environment of lipid bilayers, squalene (SQ) could be conjugated to phospholipids in the formation of liposomes. The effect of membrane composition and concentrations on the degradation of liposomes prepared via the extrusion method was investigated. Liposomes were prepared using a mixture of SQ, cholesterol (CH) and Tween80 (TW80). Based on the optimal conditions, liposome batches were prepared in the absence and presence of SQ. Their physicochemical and stability behavior were evaluated as a function of liposome constituent. From the optimization study, the liposomal formulation containing 5% (w/w) mixed soy lecithin (ML), 0.5% (w/w) SQ, 0.3% (w/w) CH and 0.75% (w/w) TW80 had optimal physicochemical properties and displayed a unilamellar structure. Liposome prepared using the optimal formulation had a low particle size (158.31 ± 2.96 nm) and acceptable %increase in the particle size (15.09% ± 3.76%) and %trolox equivalent antioxidant capacity (%TEAC) loss (35.69% ± 0.72%) against UV light treatment (280-320 nm) for 6 h. The interesting outcome of this research was the association of naturally occurring substance SQ for size reduction without the extra input of energy or mechanical procedures, and improvement of vesicle stability and antioxidant activity of ML-based liposome. This study also demonstrated that the presence of SQ in the membrane might increase the acyl chain dynamics and decrease the viscosity of the dispersion, thereby limiting long-term stability of the liposome.
In our previous study, a novel alginate-based bilayer film for slow-release wound dressings was successfully developed. We found that alginate alone yielded poor films; however, the addition of gelatine had significantly enhanced the drug dispersion as well as the physical properties. Here, an investigation of the drug-polymer interactions in the bilayer films was carried out. Drug content uniformity test and microscopy observation revealed that the addition of gelatine generated bilayer films with a homogenous drug distribution within the matrix. The FTIR and XRD data showed an increase in film crystallinity which might infer the presence of drug-polymer crystalline microaggregates in the films. DSC confirmed the drug-polymer interaction and indicated that the gelatine has no effect on the thermal behaviour of the microaggregates, suggesting the compatibility of the drug and excipients in the bilayer films. In conclusion, the addition of gelatine can promote homogenous dispersion of hydrophobic drugs in alginate films possibly through the formation of crystalline microaggregates.
In this work, a novel solvent, deep eutectic solvent (DES) was applied to examine its effectiveness in pretreating OPEFB. Three types of DESs, i.e. choline chloride-lactic acid (ChCl-LA), choline chloride-urea (ChCl-U) and choline chloride-glycerol (ChCl-G) were investigated. The pretreatment performance was based on cellulose digestibility, structural and morphology changes. At molar ratio of 1:2, ChCl-LA attained the highest reducing sugars yield of 20.7%, followed by ChCl-G (20.0%) and ChCl-U (16.9%). FT-IR and SEM results further confirmed the outstanding ability of ChCl-LA due of its ability in cellulose, hemicellulose and lignin disruption, exposing its cellulose fraction to enzymatic hydrolysis. ChCl-LA is also more favorable compare to acid and alkaline solvents as it could prevent sugars loss, use of expensive corrosion resistant equipment and ease products separation.
The carboxymethyl sago pulp (CMSP) with a degree of substitution of 0.4% was synthesized from sago waste. The CMSP beads with an average diameter of 3.1-4.8 mm were formed by aluminium chloride gelation as well as further cross-linked by irradiation. To evaluate colon targeted release, a model drug, 5-aminosalicylic acid (5-ASA) was encapsulated in CMSP beads. Fourier-transform infrared spectroscopy and X-ray diffraction studies indicated intact and amorphous nature of entrapped drug. A pH dependent drug release was observed, and about 90% of the drug was released only at pH 7.4 over 9 h. Irradiated beads were resisted the drug release in an acidic environment at a higher extent than non-irradiated beads. The drug release from 6% (w/w) of 5-ASA loaded bead followed zero order, whereas, 15 and 22% loaded beads followed first order. The release exponent n value suggests non-fickian transport of 5-ASA from the beads.
A series of poly(urea-formaldehyde) (PUF) microcapsules filled with dicyclopentadiene (DCPD) was successfully prepared by in situ polymerization. The effect of diverse process parameters and ingredients on the morphology of the microcapsules was observed by SEM, optical microscopy (OM) and digital microscopy. Different techniques for the characterization of the chemical structure and the core content were considered such as FT-IR and 1H-NMR as well as the characterization of thermal properties by DSC. High yields of free flowing powder of spherical microcapsules were produced. The synthesized microcapsules can be incorporated into another polymeric host material. In the event the host material cracks due to excessive stress or strong impact, the microcapsules would rupture to release the DCPD, which could polymerize to repair the crack.
Nanocellulose prepared from the natural material has a promising wide range of opportunities to obtain the superior material properties towards various end-products. In this research, commercially available natural cotton was treated with aqueous sodium hydroxide solution to eliminate the hemicellulose and lignin, then cellulose was collected. The collected cellulose was subjected to acid hydrolysis using sulfuric acid to obtain nanocellulose. The prepared nanocellulose was further characterized with the aid of Fourier transform infrared spectroscopy, X-ray diffraction and Scanning Electron Microscopy to elucidate the chemical structure, crystallinity and the morphology.
The structure of (E)-1-(4-Bromophenyl)-3-(napthalen-2-yl)prop-2-en-1-one (C19H13BrO) crystallized in the triclinic system of P-1 space group. The unit cell dimensions are: a=5.8944 (9)Å, b=7.8190 (12)Å, c=16.320 (2)Å, α=102.4364 (19)°, β=95.943 (2)°, γ=96.274 (2)° and Z=2. The physical properties of this compound was determined by the spectroscopic methods (FTIR and (1)H and (13)C NMR). Quantum chemical investigations have been employed to investigate the structural and spectral properties. The molecular structure, vibrational assignments, (1)H and (13)C NMR chemical shift values, non-linear optical (NLO) effect, HOMO-LUMO analysis and natural bonding orbital (NBO) analysis were calculated using HF and DFT/B3LYP methods with 6-311++G(d,p) basis set in the ground state. The results show that the theoretical calculation of the geometrical parameters, vibrational frequencies and chemical shifts are comparable with the experimental data. The crystal structure is influenced and stabilized by weak C-H⋯π interactions connecting the molecules into infinite supramolecular one dimensional ladder-like arrangement. Additionally, this compound is evaluated for their antibacterial activities against gram positive and gram negative strains using a micro dilution procedure and shows activities against a panel of microorganisms.
Plant leaf litter has a major role in the structure and function of soil ecosystems as it is associated with nutrient release and cycling. The present study is aimed to understand how well the decomposing leaf litter kept soil organic carbon and nitrogen levels stable during an incubation experiment that was carried out in a lab setting under controlled conditions and the results were compared to those from a natural plantation. In natural site soil samples, Anacardium. occidentale showed a higher value of organic carbon at surface (1.14%) and subsurface (0.93%) and Azadirachta. indica exhibited a higher value of total nitrogen at surface (0.28%) and subsurface sample (0.14%). In the incubation experiment, Acacia auriculiformis had the highest organic carbon content initially (5.26%), whereas A. occidentale had the highest nitrogen level on 30th day (0.67%). The overall carbon-nitrogen ratio showed a varied tendency, which may be due to dynamic changes in the complex decomposition cycle. The higher rate of mass loss and decay was observed in A. indica leaf litter, the range of the decay constant is 1.26-2.22. The morphological and chemical changes of soil sample and the vermicast were substantained using scanning electron microscopy (SEM) and Fourier transmission infrared spectroscopy (FT-IR).
The current study reports the synthesis of sustainable nano-hydroxyapatite (nHAp) using a wet chemical precipitation approach. The materials used in the green synthesis of nHAp were obtained from environmental biowastes such as HAp from eggshells and pectin from banana peels. The physicochemical characterization of obtained nHAp was carried out using different techniques. For instance, X-ray diffractometer (XRD) and FTIR spectroscopy were used to study the crystallinity and synthesis of nHAp respectively. In addition, the morphology and elemental composition of nHAP were studied using FESEM equipped with EDX. HRTEM showed the internal structure of nHAP and calculated its grain size which was 64 nm. Furthermore, the prepared nHAp was explored for its antibacterial and antibiofilm activity which has received less attention previously. The obtained results showed the potential of pectin-bound nHAp as an antibacterial agent for various biomedical and healthcare applications.