Recently, the oxidative behavior of methotrexate (MTX) anticancer drug is highly demanded, due to its side effects on healthy cells, despite being a very challenging task. In this study, we have prepared porous NiO material using sodium sulfate as an electronic disorder reagent by hydrothermal method and found it highly sensitive and selective for the oxidation of MTX. The synthesized NiO nanostructures were characterized by scanning electron microscope (SEM) and X-ray diffraction (XRD) techniques. These physical characterizations delineated the porous morphology and cubic crystalline phase of NiO. Different electrochemical approaches have been utilized to determine the MTX concentrations in 0.04 M Britton–Robinson buffer (BRB) at pH 2 using glassy carbon electrode (GCE)-modified with electronically disordered NiO nanostructures. The linear range for MTX using cyclic voltammetry (CV) was found to be from 5 to 30 nM, and the limit of detection (LOD) and limit of quantification (LOQ) were 1.46 nM and 4.86 nM, respectively, whereas the linear range obtained via linear sweep voltammetry (LSV) was estimated as 15–90 nM with LOD and LOQ of 0.819 nM and 2.713 nM, respectively. Additionally, amperometric studies revealed a linear range from 10 to70 nM with LOD and LOQ of 0.1 nM and 1.3 nM, respectively. Importantly, MTX was successfully monitored in pharmaceutical products using the standard recovery method. Thus, the proposed approach for the synthesis of active metal oxide materials could be sued for the determination of other anticancer drugs in real samples and other biomedical applications.
The monitoring of hypertension drugs is very critical and important to sustain a healthy life. In this study, we have synthesized nickel oxide (NiO) nanostructures using potassium dichromate as surface modifying agent by hydrothermal method. These NiO nanostructures were found highly active for the oxidation of ADB besylate (ADB). The unit cell structure and morphology were investigated by scanning electron microscopy (SEM) and powder X‐ray diffraction (XRD) techniques. The SEM study has confirmed the nano sheet like morphology and XRD analysis has described the cubic unit arrays of NiO. After the physical characterization, NiO nanostructures were used to modify the surface of glassy carbon electrode (GCE) by drop casting method. Then cyclic voltammetry (CV) was used to characterize the electrochemical activity of NiO nanostructures in the0.1 M phosphate buffer solution of pH 10.0 and a well resolved oxidation peak was identified at 0.70 V. The linear range for the NiO nanostructures was observed from 20–90 nM with a regression coefficient of 0.99 using CV. The calculated limit of detection (LOD) was 2.125 nM and the limit of quantification (LOQ) was 4.08 nM. Further to validate the CV calibration plot, an amperometry experiment was performed on the NiO nanostructures and sensors exhibited a linear range of 10 nM to 115 nM with LOD of 1.15 nM. The proposed approach was successfully used for the determination of ADB from commercial tablets and it reveals that the sensor could be capitalized to monitor ADB concentrations from pharmaceutical products. The use of potassium dichromate as a surface modifying agent for the metal oxide nanostructures may be of great interest to manipulate their crystal and surface properties for the extended range of biomedical and energy related applications.
Keywords: Fried vermicelli Soxhlet extraction Fatty acids GC-MS FTIR ChemometricsIntroduction. Snacks are common food throughout the world including subcontinent. Most of the snack foods are prepared in oil and fat. In current study, fried vermicelli (common snack food) was selected to evaluate the quality as it is largely consumed in many countries.Materials and methods. Fried vermicelli was subjected for the extraction of total oil by applying Soxhlet extraction method using hexane as a solvent. Fatty acid composition of extracted fried vermicelli oil was checked on GC-MS. Similarly, FTIR spectroscopy was also used to record the spectra of same oil for the development of simple methodology to quantify fatty acid groups and ratios.Results and discussion. High percentage of oil content was observed in all fried vermicelli samples (19.77-32.99%). Fatty acid composition exposed that palmitic (34.6-47.5%), stearic (4.76 to 10.6%), oleic (27.2-37.0%) and elaidic acid (12.0-24.3%) were predominant fatty acids among saturated and monounsaturated fatty acids. While polyunsatured fatty acids were observed comparatively in less quantity in fried vermicelli (0.66 to 5.99 %). The presence of higher trans fatty acids indicated that fried vermicelli was prepared in hydrogenated oil. Fatty acid ratios of some important groups were observed in the range of 0.72-1.92 SFA/UFA, 0.013-0.130 cis PUFA/SFA, 0.1 to 1.81 trans FA/cis FA, 0.01 to 0.097 cis PUFA/SFA + TFA, 27.7-37.05 cis MUFA + cis PUFA/SFA + TFA. The obtained results of groups and ratios by GC-MS were used to develop different calibration models for the quantification of fatty acid groups and fatty acid ratios using PLS chemometric approach. The developed PLS models using selected wavelength regions showed higher correlations (>0.99) with GC-MS results.Conclusions. It can be concluded that quality of fried vermicelli marketed locally is worrisome matter for the consumers and quality control authorities. FTIR provided complete profiling of groups and ratios in fried vermicelli very accurately with negligible difference in the results. The proposed methodology serves as a rapid and simple quantitative tool for quality evaluation of major groups and ratios.
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