Testosterone thiosemicarbazone, L and its nickel (II) complex 1 were synthesized and characterized by using FTIR, CHN, (1)H NMR, and X-ray crystallography. X-ray diffraction study confirmed the formation of L from condensation of testosterone and thiosemicarbazide. Mononuclear complex 1 is coordinated to two Schiff base ligands via two imine nitrogens and two tautomeric thiol sulfurs. The cytotoxicity of both compounds was investigated via MTT assay with cisplatin as positive reference standard. L is more potent towards androgen-dependent LNCaP (prostate) and HCT 116 (colon). On the other hand, complex 1, which is in a distorted square planar environment with L acting as a bidentate NS-donor ligand, is capable of inhibiting the growth of all the cancer cell lines tested, including PC-3 (prostate). It is noteworthy that both compounds are less toxic towards human colon cell CCD-18Co. The intrinsic DNA binding constant (Kb) of both compounds were evaluated via UV-Vis spectrophotometry. Both compounds showed Kb values which are comparable to the reported Kb value of typical classical intercalator such as ethidium bromide. The binding constant of the complex is almost double compared with ligand L. Both compounds were unable to inhibit the action topoisomerase I, which is the common target in cancer treatment (especially colon cancer). This suggest a topoisomerase I independent-cell death mechanism.
The removal of Ni(II) from aqueous solution by magnetic nanoparticles prepared and impregnated onto tea waste (Fe(3)O(4)-TW) from agriculture biomass was investigated. Magnetic nanoparticles (Fe(3)O(4)) were prepared by chemical precipitation of a Fe(2+) and Fe(3+) salts from aqueous solution by ammonia solution. These magnetic nanoparticles of the adsorbent Fe(3)O(4) were characterized by surface area (BET), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM) and Fourier Transform-Infrared Spectroscopy (FT-IR). The effects of various parameters, such as contact time, pH, concentration, adsorbent dosage and temperature were studied. The kinetics followed is first order in nature, and the value of rate constant was found to be 1.90×10(-2) min(-1) at 100 mg L(-1) and 303 K. Removal efficiency decreases from 99 to 87% by increasing the concentration of Ni(II) in solution from 50 to 100 mg L(-1). It was found that the adsorption of Ni(II) increases by increasing temperature from 303 to 323 K and the process is endothermic in nature. The adsorption isotherm data were fitted to Langmuir and Freundlich equation, and the Langmuir adsorption capacity, Q°, was found to be (38.3)mgg(-1). The results also revealed that nanoparticle impregnated onto tea waste from agriculture biomass, can be an attractive option for metal removal from industrial effluent.
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.
The technique of Fourier transform infrared spectroscopy is widely used to generate spectral data for use in the detection of food contaminants. Monochloropropanediol (MCPD) is a refining process-induced contaminant that is found in palm-based fats and oils. In this study, a chemometric approach was used to evaluate the relationship between the FTIR spectra and the total MCPD content of a palm-based cooking oil. A total of 156 samples were used to develop partial least squares regression (PLSR), artificial neural network (nnet), average artificial neural network (avNNET), random forest (RF) and cubist models. In addition, a consensus approach was used to generate fusion result consisted from all the model mentioned above. All the models were evaluated based on validation performed using training and testing datasets. In addition, the box plot of coefficient of determination (R2), root mean square error (RMSE), slopes and intercepts by 100 times randomization was also compared. Evaluation of performance based on the testing R2 and RMSE suggested that the cubist model predicted total MCPD content with the highest accuracy, followed by the RF, avNNET, nnet and PLSR models. The overfitting tendency was assessed based on differences in R2 and RMSE in the training and testing calibrations. The observations showed that the cubist and avNNET models possessed a certain degree of overfitting. However, the accuracy of these models in predicting the total MCPD content was high. Results of the consensus model showed that it slightly improved the accuracy of prediction as well as significantly reduced its uncertainty. The important variables derived from the cubist and RF models suggested that the wavenumbers corresponding to the MCPDs originated from the -CH=CH2 or CH=CH (990-900 cm-1) and C-Cl stretch (800-700 cm-1) regions of the FTIR spectrum data. In short, chemometrics in combination with FTIR analysis especially for the consensus model represent a potential and flexible technique for estimating the total MCPD content of refined vegetable oils.
Hermetia illucens larvae by nature are a decomposer which fed on organic wastes. This study explores the potential of producing biodiesel using lipids from H. illucens larvae. Three types of organic wastes (sewage sludge, fruit waste and palm decanter cake from oil palm mill) were selected based on considerable generation and disposal concern in the area of study as well as lack of investigations as feed for Hermetia illucens larvae in current literatures. Growth rate of the larvae was determined with studying the changes in the biomass per day. H. illucens larvae fed with fruit waste and palm decanter cake have shown growth rates of 0.52±0.02 and 0.23±0.09 g d(-1), respectively. No positive sign of growth were observed in the larvae fed with treated sewage sludge (-0.04±0.01 g d(-1)). Biodiesel as fatty acid methyl ester (FAME) was synthesized by transesterification of the larvae lipid using sulphuric acid as catalyst in methanol. FAME produced was ascertained using ATR-FTIR spectroscopy and GC-MS. The main compositions of fatty acid were found to be C12:0, C16:0 and C18:1n9c. Fatty acid composition of C12:0 fed with fruit waste, sewage sludge and palm decanter was found to be most abundant in the larvae lipid. The amount of C12:0 obtained was 76.13%, 58.31% and 48.06%, respectively. In addition, fatty acid of C16:0 was attained at 16.48% and 25.48% fed with sewage sludge and palm decanter, respectively. Based on the findings, FAME derived from larvae lipids is feasible to be used for biodiesel production.
A new sesquiterpenoid, malayscaphiol (1), and three known compounds, lupeol (2), lupenone (3) and stigmasterol (4), were isolated from the methanolic extract of the stem bark of Scaphium macropodum. The structures of the isolated compounds were determined using several spectroscopic methods, including UV-vis, FT-IR, 1D and 2D NMR, and mass spectrometer. Major isolated compounds were assayed for cytotoxicity and anti-acetylcholinesterase activities. The chemotaxonomy significance of this plant was also discussed.
The effects of microwave on drug release properties of pectin films carrying sulfanilamide (SN-P), sulfathiazole (ST-P) and sulfamerazine (SM-P) of high to low aqueous solubilities were investigated. These films were prepared by solvent evaporation technique and treated by microwave at 80 W for 5-40 min. Their profiles of drug dissolution, drug content, matrix interaction and matrix crystallinity were determined by drug dissolution testing, drug content assay, differential scanning calorimetry, X-ray diffractometry and scanning electron microscopy techniques. Microwave induced an increase in matrix amorphousness but lower drug release propensity with a greater retardation extent in SN-P films, following a rise in strength of matrix interaction. A gain in amorphous structure does not necessarily increase the drug release of film. Microwave can possibly retard drug release of pectin film carrying water-soluble drug through modulating its state of matrix interaction.
The applicability of microwave non-destructive testing (NDT) technique in characterization of matrix property of pharmaceutical films was investigated. Hydroxypropylmethylcellulose and loratadine were selected as model matrix polymer and drug, respectively. Both blank and drug loaded hydroxypropylmethylcellulose films were prepared using the solvent-evaporation method and were conditioned at the relative humidity of 25, 50 and 75% prior to physicochemical characterization using microwave NDT technique as well as ultraviolet spectrophotometry, differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FT-IR) techniques. The results indicated that blank hydroxypropylmethylcellulose film exhibited a greater propensity of polymer-polymer interaction at the O-H and C-H domains of the polymer chains upon conditioned at a lower level of relative humidity. In the case of loratadine loaded films, a greater propensity of polymer-polymer and/or drug-polymer interaction via the O-H moiety was mediated in samples conditioned at the lower level of relative humidity, and via the C-H moiety when 50% relative humidity was selected as the condition for sample storage. Apparently, the absorption and transmission characteristics of both blank and drug loaded films for microwave varied with the state of polymer-polymer and/or drug-polymer interaction involving the O-H and C-H moieties. The measurement of microwave NDT test at 8GHz was sensitive to the chemical environment involving O-H moiety while it was greatly governed by the C-H moiety in test conducted at a higher frequency band of microwave. Similar observation was obtained with respect to the profiles of microwave NDT measurements against the state of polymer-polymer and/or drug-polymer interaction of hydroxypropylmethylcellulose films containing chlorpheniramine maleate. The microwave NDT measurement is potentially suitable for use as an apparent indicator of the state of polymer-polymer and drug-polymer interaction of the matrix.
Pressure ulcers are commonly associated with microbial infections on the wounds which require an effective wound dressing for treatment. Thus far, the available silver dressing has shown tremendous result, however, it may cause argyria and complicate the internal organ function. Hence, our study aims to develop and characterize phomopsidione-loaded chitosan-polyethylene glycol nanocomposite hydrogel (C/PEG/Ph) as an antimicrobial dressing. Physically, the C/PEG/Ph hydrogel demonstrated a uniform light blue color, soft, flexible, and elastic, with no aggregation form. The evaluation via Fourier Transform Infrared (FTIR) exposed the C/PEG/Ph hydrogel has a notable shift towards lower frequency at 1600 and 1554 cm-1. For drug release test, the phomopsidione attained plateau at 24 h, with a total release of 67.9 ± 6.4% from the C/PEG/Ph hydrogel. There was a null burst release effect discovered throughout the experimental period. The C/PEG/Ph hydrogel showed significant results against all 4 Gram-negative bacteria and 1 yeast, with 99.99-100% reduction of microbial growth. The findings revealed that the C/PEG/Ph hydrogel can potentially act as an antimicrobial dressing for pressure ulcers.
Fennel seed spent (FSS)-an inexpensive nutraceutical industrial spent has been used as an efficient biosorbent for the removal of Congo red (CR) from aqueous media. Results show that the conditions for maximum adsorption would be pH 2-4 and 30°C were ideal for maximum adsorption. Based on regression fitting of the data, it was determined that the Sips isotherm (R2 = 0.994, χ2 = 0.5) adequately described the mechanism of adsorption, suggesting that the adsorption occurs homogeneously with favorable interaction between layers with favorable interaction between layers. Thermodynamic analysis showed that the adsorption is favorable (negative values for ΔG°) and endothermic (ΔH° = 12-20 kJ mol-1) for initial dye concentrations of 25, 50, and 100 ppm. The low ΔH° value indicates that the adsorption is a physical process involving weak chemical interactions like hydrogen bonds and van der Waals interactions. The kinetics revealed that the adsorption process showed pseudo-second-order tendencies with the equal influence of intraparticle as well as film diffusion. The scanning electron microscopy images of FSS show a highly fibrous matrix with a hierarchical porous structure. The Fourier transform infrared spectroscopy analysis of the spent confirmed the presence of cellulosic and lignocellulosic matter, giving it both hydrophilic and hydrophobic properties. The investigations indicate that FSS is a cost-effective and efficient biosorbent for the remediation of toxic CR dye.
The most effective treatment for spinal tuberculosis was by eliminating the tuberculosis bacteria and replacing the infected bone with the bone graft to induce the healing process. This study aims to synthesize and characterize nanohydroxyapatite-gelatin-based injectable bone substitute (IBS) with addition of streptomycin. The IBS was synthesized by mixing nanohydroxyapatite and 20 w/v% gelatin with ratio of 40:60, 45:55, 50:50, 55:45, 60:40, 65:35, 70:30, and 75:25 ratio and streptomycin addition as antibiotic agent. The mixture was added by hydroxypropyl methylcellulose as suspending agent. FTIR test showed that there was a chemical reaction occurring in the mixture, between the gelatin and streptomycin. The result of injectability test showed that the highest injectability of the IBS sample was 98.64% with the setting time between 30 minutes and four hours after injection on the HA scaffold that represents the bone cavity and coat the pore scaffold. The cytotoxicity test result showed that the IBS samples were nontoxic towards BHK-21 fibroblast cells and human hepatocyte cells since the viability cell was more than 50% with significant difference (p-value<0.05). The acidity of the IBS was stable and it was sensitive towards Staphylococcus aureus with significantly difference (p-value<0.05). The streptomycin release test showed that the streptomycin could be released from the IBS-injected bone scaffold with release of 2.5% after 4 hours. All the results mentioned showed that IBS was suitable as a candidate to be used in spinal tuberculosis case.
Introduction: : Ginseng is a type of traditional medicine that has been used for thousand years to treat various dis- eases and has been proven effective in treating cardiovascular diseases. Incorporation of polyaniline (PANI) which is a type of conductive polymer together with ginseng into poly(lactic-co-glycolic acid) (PLGA) microcapsules is neces- sary for the treatment of cardiovascular diseases as the polymer will control drug release and the electroconductivity of PANI is beneficial on myocardium cells. Methods: Therefore, this project involved the encapsulation of ginseng inside PLGA/PANI microcapsules. The encapsulation of ginseng inside the microcapsules was verified through the identification of chemical composition of ginseng, PLGA and PANI using attenuated total reflectance-Fourier trans- form infrared spectroscopy (ATR-FTIR). Results: The results of scanning electron microscope (SEM) showed the formation of microspheres where the microcapsule size was decreased from 3.14±1.87 μm to 1.98±1.30 μm as the concentration of PANI increased. The distribution of microcapsules size was more homogeneous in the high con- centration of PANI as been determined through the histogram analysis. In addition, the fluorescence analysis demon- strated the efficiency of ginseng encapsulation inside PLGA/PANI microcapsules through the appearance of stained ginseng inside the microcapsules. Conclusion: As a conclusion, the ginseng was successfully encapsulated within PLGA/PANI microcapsules that will be beneficial in drug delivery application, specifically in the cardiovascular area.
This work is aimed to develop a biocompatible, bactericidal and mechanically stable biomaterial to overcome the challenges associated with calcium phosphate bioceramics. The influence of chemical composition on synthesis temperature, bioactivity, antibacterial activity and mechanical stability of least explored calcium silicate bioceramics was studied. The current study also investigates the biomedical applications of rankinite (Ca3Si2O7) for the first time. Sol-gel combustion method was employed for their preparation using citric acid as a fuel. Differential thermal analysis indicated that the crystallization of larnite and rankinite occurred at 795 °C and 1000 °C respectively. The transformation of secondary phases into the desired product was confirmed by XRD and FT-IR. TEM micrographs showed the particle size of larnite in the range of 100-200 nm. The surface of the samples was entirely covered by the dominant apatite phase within one week of immersion. Moreover, the compressive strength of larnite and rankinite was found to be 143 MPa and 233 MPa even after 28 days of soaking in SBF. Both samples prevented the growth of clinical pathogens at a concentration of 2 mg/mL. Larnite and rankinite supported the adhesion, proliferation and osteogenic differentiation of hBMSCs. The variation in chemical composition was found to influence the properties of larnite and rankinite. The results observed in this work signify that these materials not only exhibit faster biomineralization ability, excellent cytocompatibility but also enhanced mechanical stability and antibacterial properties.
Siliceous mesoporous molecular sieve (Si-MCM-41) material with highly ordered hexagonal pore arrangement was synthesized at 373 K for 8-days duration by hydrothermal method, dried at 393 K and calcined at 823 K in N2 atmosphere. The calcined Si-MCM-41 was later functionalized with 10-50 wt. % monoethanolamine (MEA) by impregnation method and dried in vacuum at 343 K. The MEA-Si-MCM-41 samples were characterized for their physicochemical properties with FTIR, XRD, TGA, HRTEM, FESEM, BET and elemental analysis. XRD results showed that the intensity of the characteristic peaks of Si-MCM-41 reduces with increasing loading of MEA indicating that the MEA molecules are loaded in the pores as well as on the surface of Si-MCM-41. The appearance of FTIR peaks corresponding to N-H, C-N and C-H bonds suggested that Si-MCM-41 has been functionalized with MEA. The presence of Si-O-Si peaks in FTIR spectra of MEA-Si-MCM-41 samples indicates that the hexagonal pore arrangement remains intact and this is supported by HRTEM images. FESEM images show that MEA-Si-MCM-41 samples became agglomerated with increase loading of MEA. TGA analyses show that the MEA-Si-MCM-41 samples are thermally stable up to 528 K. N2 adsorption-desorption isotherms show that the textural properties of Si-MCM-41 material slowly change from a mesoporous material to non-porous material as the MEA loading increases due to pore filling effect during functionalization with MEA. Detection of N, C and H by elemental analysis confirms the presence of MEA in MEA-Si-MCM-41 samples.
Scaffolds supplemented with naturally derived materials seem to be a good choice in bone tissue engineering. This study aims to develop polyurethane (PU) nanofibers added with ylang ylang (YY) and zinc nitrate (ZnNO3) using the electrospinning method. Field emission scanning electron microscopy (FESEM) images showed that the diameter of the PU nanofibers (869 ± 122 nm) was reduced with the addition of YY and ZnNO3 (PU/YY-467 ± 132 nm and PU/YY/ZnNO3-290 ± 163 nm). Fourier transform infrared (FTIR), a thermal gravimetric analysis (TGA) and an X-ray diffraction (XRD) analysis confirmed the interactions between PU with YY and ZnNO3. In addition, a thermal gravimetric analysis (TGA) study revealed the improved thermal stability for PU/YY and a slight reduction in the thermal stability for PU/YY/ZnNO3. A tensile test indicated that the addition of YY and ZnNO3 (PU/YY-12.32 MPa and PU/YY/ZnNO3-14.90 MPa) improved the mechanical properties of the pristine PU (6.83 MPa). The electrospun PU/YY (524 nm) and PU/YY/ZnNO3 (284 nm) showed a reduced surface roughness when compared with the pristine PU (776 nm) as depicted in the atomic force microscopy (AFM) analysis. The addition of YY and ZnNO3 improved the anticoagulant and biocompatibility nature of the pristine PU. Furthermore, the bone mineralization study depicted the improved calcium deposition in the fabricated composites (PU/YY-7.919% and PU/YY/ZnNO3-10.150%) compared to the pristine PU (5.323%). Hence, the developed composites with desirable physico-chemical properties, biocompatibility and calcium deposition can serve as plausible candidates for bone tissue engineering.
Cardiovascular application of nanomaterial's is of increasing demand and its usage is limited by its mechanical and blood compatible properties. In this work, an attempt is made to develop an electrospun novel nanocomposite loaded with basil oil and titanium dioxide (TiO2) particles. The composite material displayed increase in hydrophobic and reduced fiber diameter compared to the pristine polymer. Fourier transform infrared spectroscopy results showed the interaction of the pristine polymer with the added substances. Thermal analysis showed the increased onset degradation, whereas the mechanical testing portrayed the increased tensile strength of the composites. Finally, the composite delayed the coagulation times and also rendered safe environment for red blood cells signifying its suitability to be used in contact with blood. Strikingly, the cellular toxicity of the developed composite was lower than the pristine polymer suggesting its compatible nature with the surrounding tissues. With these promising characteristics, developed material with enhanced physicochemical properties and blood compatibility can be successfully utilized for cardiac tissue applications.
This study was conducted to prepare a mixed matrix membrane (MMM) and to test the performance of the prepared MMM for CO2 and CH4 gas separation. MMM containing polyethersulfone (PES) and multi-walled carbon nanotubes (MWCNTs) was prepared by a dry-wet phase inversion technique using a pneumatically-controlled membrane casting machine. The surface modification was performed on MWCNTs in order to enhance the selectivity of CO2/CH4. The surface modification of MWCNTs using chemical and physical approaches has been adopted. Mixed acid (HNO3/H2SO4) and β-CD were used for chemical and physical approaches, respectively. Effects of surface modification on MWCNTs/PES MMM were investigated. MWCNTs/PES MMMs were characterised using scanning electron microscopy (SEM), the Fourier Transform Infrared (FT-IR) spectroscopy and pure gas permeation test. The permeability and selectivity, which are the parameters describing membrane performance were calculated via the data obtained from pure gas permeation test with the feed pressure difference from 3 to 7 bars. In this study, surface modified MWCNTs/PES MMM using mixed acid and β-CD has successfully enhanced the CO2/CH4 selectivity by 40.6% compared to that of neat PES.
Conductive materials are potential candidates for developing bone tissue engineering scaffolds as they are nontoxic and can enhance bone tissue regeneration. Their bioactivity can be enhanced by depositing biomineralization in simulated body fluid (SBF). In the current study, a composite electrospun membrane made up of poly(lactic) acid, poly(3-hydroxybutyrate-co-3-hydroxyvalerate), and hydroxyapatite was fabricated using an electrospinning method. The fabricated membranes were dip-coated with a conductive polymer solution, poly(3,4-ethylenedioxythiophene) poly(4-styrenesulfonate), to induce conductivity. Characterization of the membranes based on characteristics such as morphology, chemical bonding, and wettability was conducted using scanning electron microscopy, field emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, attenuated total reflectance Fourier transform infrared spectroscopy, and contact angle measurement. From the results, biomineralization of both coated and noncoated composite membranes was observed on the surface of nanofibers after 21 days in SBF. The membranes provide a superhydrophilic surface as shown by the contact angle. In conclusion, this biomimetic electrospun composite membrane could be used to further support cell growth for bone tissue engineering application.
Considering the important factor of bioactive nanohydoxyapatite (nHA) to enhance osteoconductivity or bone-bonding capacity, nHA was incorporated into an electrospun polycaprolactone (PCL) membrane using electrospinning techniques. The viscosity of the PCL and nHA/PCL with different concentrations of nHA was measured and the morphology of the electrospun membranes was compared using a field emission scanning electron microscopy. The water contact angle of the nanofiber determined the wettability of the membranes of different concentrations. The surface roughness of the electrospun nanofibers fabricated from pure PCL and nHA/PCL was determined and compared using atomic force microscopy. Attenuated total reflectance Fourier transform infrared spectroscopy was used to study the chemical bonding of the composite electrospun nanofibers. Beadless nanofibers were achieved after the incorporation of nHA with a diameter of 200-700 nm. Results showed that the fiber diameter and the surface roughness of electrospun nanofibers were significantly increased after the incorporation of nHA. In contrast, the water contact angle (132° ± 3.5°) was reduced for PCL membrane after addition of 10% (w/w) nHA (112° ± 3.0°). Ultimate tensile strengths of PCL membrane and 10% (w/w) nHA/PCL membrane were 25.02 ± 2.3 and 18.5 ± 4.4 MPa. A model drug tetracycline hydrochloride was successfully loaded in the membrane and the membrane demonstrated good antibacterial effects against the growth of bacteria by showing inhibition zone for E. coli (2.53 ± 0.06 cm) and B. cereus (2.87 ± 0.06 cm).
White rice husk ash (RHA), an agriculture waste containing crystalline tridymite and alpha-cristobalite, was used as a silica source for zeolite Beta synthesis. The crystallization of zeolite Beta from RHA at 150 degrees C in the presence of tetraethylammonium hydroxide was monitored by XRD, FTIR and (29)Si MAS NMR techniques. It was found that zeolite Beta started to form after 12h and the complete crystallization of zeolite Beta phase was achieved after 2d. XRD, (29)Si MAS NMR and solid yield studies indicate that the transformation mechanism of silica present in RHA to zeolite Beta involves dissolution of the ash, formation of an amorphous aluminosilicate after 6h of crystallization, followed by dissolution in the mother liquor and final transformation to pure zeolite Beta crystals.