Rohana Adnan

Enantioselective analysis of ofloxacin and ornidazole in pharmaceutical formulations by capillary electrophoresis using single chiral selector and computational calculation of their inclusion complexes

A capillary electrophoretic method for the separation of the enantiomers of both ofloxacin and ornidazole is described. Several parameters affecting the separation were studied, including the type and concentration of chiral selector, buffer pH, voltage and temperature. Good chiral separation of the racemic mixtures was achieved in less than 16 min with resolution factors Rs=5.45 and 6.28 for ofloxacin and ornidazole enantiomers, respectively. Separation was conducted using a bare fused-silica capillary and a background electrolyte (BGE) of 50 mM H(3)PO(4)-1 M tris solution; pH 1.85; containing 30 mg mL(-1) of sulfated-beta-cyclodextrin (S-beta-CD). The separation was carried out in reversed polarity mode at 25 degrees C, 18 kV, detection wavelength at 230 nm and using hydrodynamic injection for 15 s. Acceptable validation criteria for selectivity, linearity, precision, and accuracy were studied. The limits of detection (LOD) and limits of quantitation (LOQ) of the enantiomers (ofloxacin enantiomer 1 (OF-E1), ofloxacin enantiomer 2 (OF-E2), ornidazole enantiomer 1 (OR-E1) and ornidazole enantiomer 2 (OR-E2)) were (0.52, 0.46, 0.54, 0.89) and (1.59, 1.40, 3.07, 2.70) microg mL(-1), respectively. The proposed method was successfully applied to the assay of enantiomers of both ofloxacin and ornidazole in pharmaceutical formulations. The computational calculations for the enantiomeric inclusion complexes rationalized the reasons for the different migration times between the ofloxacin and ornidazole enantiomers.

Comparative study between Pap smear cytology and FTIR spectroscopy: a new tool for screening for cervical cancer

Aims: To evaluate Fourier transform infrared (FTIR) spectroscopy as new tool for screening of cervical cancer in comparison with cervical cytology. Methods: A total of 800 cervical scrapings were taken by cytobrush and placed in ThinPrep medium. The samples were dried over infrared transparent matrix. Beams of infrared light were directed at the dried samples at frequency of 4000 to 400 cm‐1. The absorption data were produced using a Spectrum BX II FTIR spectrometer. Data were compared with the reference absorption data of known samples using FTIR spectroscopy software. FTIR spectroscopy was compared with cytology (gold standard). Results: FTIR spectroscopy could differentiate normal from abnormal cervical cells in the samples examined. The sensitivity was 85%, specificity 91%, positive predictive value 19.5% and negative predictive value of 99.5%. Conclusion: This study suggests that FTIR spectroscopy could be used as an alternative method for screening for cervical cancer.

Micelle-Assisted Synthesis of Al2O3·CaO Nanocatalyst: Optical Properties and Their Applications in Photodegradation of 2,4,6-Trinitrophenol

Calcium oxide (CaO) nanoparticles are known to exhibit unique property due to their high adsorption capacity and good catalytic activity. In this work the CaO nanocatalysts were prepared by hydrothermal method using anionic surfactant, sodium dodecyl sulphate (SDS), as a templating agent. The as-synthesized nanocatalysts were further used as substrate for the synthesis of alumina doped calcium oxide (Al2O3 ·CaO) nanocatalysts via deposition-precipitation method at the isoelectric point of CaO. The Al2O3 ·CaO nanocatalysts were characterized by FTIR, XRD, TGA, TEM, and FESEM techniques. The catalytic efficiencies of these nanocatalysts were studied for the photodegradation of 2,4,6-trinitrophenol (2,4,6-TNP), which is an industrial pollutant, spectrophotometrically. The effect of surfactant and temperature on size of nanocatalysts was also studied. The smallest particle size and highest percentage of degradation were observed at critical micelle concentration of the surfactant. The direct optical band gap of the Al2O3 ·CaO nanocatalyst was found as 3.3 eV.

Optical absorption and photoluminescence studies of gold nanoparticles deposited on porous silicon.

We present an investigation on a coupled system consists of gold nanoparticles and silicon nanocrystals. Gold nanoparticles (AuNPs) embedded into porous silicon (PSi) were prepared using the electrochemical deposition method. Scanning electron microscope images and energy-dispersive X-ray results indicated that the growth of AuNPs on PSi varies with current density. X-ray diffraction analysis showed the presence of cubic gold phases with crystallite sizes around 40 to 58 nm. Size dependence on the plasmon absorption was studied from nanoparticles with various sizes. Comparison with the reference sample, PSi without AuNP deposition, showed a significant blueshift with decreasing AuNP size which was explained in terms of optical coupling between PSi and AuNPs within the pores featuring localized plasmon resonances.

Simultaneous 4-chlorophenol and nitrogen removal in moving bed sequencing batch reactors packed with polyurethane foam cubes of various sizes.

Moving bed sequencing batch reactors (MBSBRs) packed with 8% (v/v) of 8-, 27- and 64-mL polyurethane (PU) foam cubes, respectively, were investigated for simultaneous 4-chlorophenol (4-CP) and nitrogen removal at increasing 4-CP concentration. When the 4-CP concentration exceeded 300 mg L(-1), the MBSBR with 27-mL foam cubes was observed to outperform the other MBSBRs in removing 4-CP and nitrogen. The reasons were: (1) there were more biomass in inner layer of the 27-mL cubes, compared to that of the 8-mL cubes, which was more shielded from the inhibitory effect of 4-CP and (2) the 27-mL cubes were more mobile than the 64-mL cubes. Although increasing 4-CP concentration to 600 mg L(-1) resulted in incomplete removal of 4-CP in the MBSBRs, results of the batch reactor with 27-mL foam cubes showed that complete 4-CP removal within the REACT period could be achieved by increasing the packing volume to 20%.

A Structural Study of Epoxidized Natural Rubber (ENR-50) and Its Cyclic Dithiocarbonate Derivative Using NMR Spectroscopy Techniques

A structural study of epoxidized natural rubber (ENR-50) and its cyclic dithiocarbonate derivative was carried out using NMR spectroscopy techniques. The overlapping 1H-NMR signals of ENR-50 at δ 1.56, 1.68–1.70, 2.06, 2.15–2.17 ppm were successfully assigned. In this work, the 13C-NMR chemical shift assignments of ENR-50 were consistent to the previously reported work. A cyclic dithiocarbonate derivative of ENR-50 was synthesized from the reaction of purified ENR-50 with carbon disulfide (CS2), in the presence of 4-dimethylaminopyridine (DMAP) as catalyst at reflux temperature. The cyclic dithiocarbonate formation involved the epoxide ring opening of the ENR-50. This was followed by insertion of the C–S moiety of CS2 at the oxygen attached to the quaternary carbon and methine carbon of epoxidized isoprene unit, respectively. The bands due to the C=S and C–O were clearly observed in the FTIR spectrum while the 1H-NMR spectrum of the derivative revealed the peak attributed to the methylene protons had split. The 13C-NMR spectrum of the derivative further indicates two new carbon peaks arising from the >C=S and quaternary carbon of cyclic dithiocarbonate. All other 1H- and 13C-NMR chemical shifts of the derivative remain unchanged with respect to the ENR-50.

Enhancement of azo dye Acid Orange 7 removal in newly developed horizontal subsurface-flow constructed wetland.

Horizontal subsurface-flow (HSF) constructed wetland incorporating baffles was developed to facilitate upflow and downflow conditions so that the treatment of pollutants could be achieved under multiple aerobic, anoxic and anaerobic conditions sequentially in the same wetland bed. The performances of the baffled and conventional HSF constructed wetlands, planted and unplanted, in the removal of azo dye Acid Orange 7 (AO7) were compared at the hydraulic retention times (HRT) of 5, 3 and 2 days when treating domestic wastewater spiked with AO7 concentration of 300 mg/L. The planted baffled unit was found to achieve 100%, 83% and 69% AO7 removal against 73%, 46% and 30% for the conventional unit at HRT of 5, 3 and 2 days, respectively. Longer flow path provided by baffled wetland units allowed more contact of the wastewater with the rhizomes, microbes and micro-aerobic zones resulting in relatively higher oxidation reduction potential (ORP) and enhanced performance as kinetic studies revealed faster AO7 biodegradation rate under aerobic condition. In addition, complete mineralization of AO7 was achieved in planted baffled wetland unit due to the availability of a combination of aerobic, anoxic and anaerobic conditions.

Low Concentration of Silver Nanoparticles Not Only Enhances the Activity of Horseradish Peroxidase but Alter the Structure Also

Chemical synthesis of Ag-NPs was carried out using reduction method. The reduction mechanistic approach of silver ions was found to be a basic clue for the formation of the Ag-NPs. The nanoparticles were characterized by UV-vis, FT-IR and TEM analysis. We had designed some experiments in support of our hypothesis, “low concentrations of novel nanoparticles (silver and gold) increases the activity of plant peroxidases and alter their structure also”, we had used Ag-NPs and HRP as models. The immobilization/interaction experiment had demonstrated the specific concentration range of the Ag-NPs and within this range, an increase in HRP activity was reported. At 0.08 mM concentration of Ag-NPs, 50% increase in the activity yield was found. The U.V-vis spectra had demonstrated the increase in the absorbance of HRP within the reported concentration range (0.06–0.12 mM). Above and below this concentration range there was a decrease in the activity of HRP. The results that we had found from the fluorescence spectra were also in favor of our hypothesis. There was a maximum increase in ellipticity and α-helix contents in the presence of 0.08 mM concentration of Ag-NPs, demonstrated by circular dichroism (CD) spectra. Finally, incubation of a plant peroxidase, HRP with Ag-NPs, within the reported concentration range not only enhances the activity but also alter the structure.

Synthesis and characterization of fluconazole-functionalized magnetic nanoparticles as a catalyst for the synthesis of 3-aryl and 3-amino-imidazo[1,2-a]pyridines

Fluconazole was successfully immobilized on the surface of chloropropyl-modified Fe3O4–SiO2 core–shell nanoparticles and was found to exhibit unique catalytic activity for the synthesis of 3-aryl-imidazo[1,2-a]pyridines in water. This catalyst also showed great activity in a multi-component reaction for the synthesis of 3-amino-imidazo[1,2-a]pyridines under solvent-free conditions. The magnetically-recoverable catalyst was found to be capable of repeated reuse without significant loss of activity.

A new insight to the physical interpretation of activated carbon and iron doped carbon material: Sorption affinity towards organic dye

To enhance the potential of activated carbon (AC), iron incorporation into the AC surface was examined in the present investigations. Iron doped activated carbon (FeAC) material was synthesized and characterized by using surface area analysis, energy dispersive X-ray (EDX), temperature programmed reduction (TPR) and temperature programmed desorption (TPD). The surface area of FeAC (543 m(2)/g) was found to be lower than AC (1043 m(2)/g) as a result of the pores widening due to diffusion of iron particles into the porous AC. Iron uploading on AC surface was confirmed through EDX analysis, showing up to 13.75 wt.% iron on FeAC surface. TPR and TPD profiles revealed the presence of more active sites on FeAC surface. FeAC have shown up to 98% methylene blue (MB) removal from the aqueous media. Thermodynamic parameters indicated the spontaneous and exothermic nature of the sorption processes.