Pharmacological assessment of Co3O4, CuO, NiO and ZnO nanoparticles via antibacterial, anti-biofilm and anti-quorum sensing activities.

Infectious diseases have risen dramatically as a result of the resistance of many common antibiotics. Nanotechnology provides a new avenue of investigation for the development of antimicrobial agents that effectively combat infection. The combined effects of metal-based nanoparticles (NPs) are known to have intense antibacterial activities. However, a comprehensive analysis of some NPs regarding these activities is still unavailable. This study uses the aqueous chemical growth method to synthesize Co3O4, CuO, NiO and ZnO NPs. The prepared materials were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction techniques. The antibacterial activities of NPs were tested against Gram-positive and Gram-negative bacteria using the microdilution method, such as the minimum inhibitory concentration (MIC) method. The best MIC value among all the metal oxide NPs was 0.63 against Staphylococcus epidermidis ATCC12228 through ZnO NPs. The other metal oxide NPs also showed satisfactory MIC values against different test bacteria. In addition, the biofilm inhibition and antiquorum sensing activities of NPs were also examined. The present study presents a novel approach for the relative analysis of metal-based NPs in antimicrobial studies, demonstrating their potential for bacteria removal from water and wastewater.

Selective oxidation of amaranth dye in soft drinks through tin oxide decorated reduced graphene oxide nanocomposite based electrochemical sensor.

The recent studies evaluated the extensive exploitation of azo dyes as food colorant to improve the texture of food to turn the food to be very attractive. The heavy consumption of the food colorants by the food industries in commonly consumed beverages especially in the soft drinks may become the cause of certain suspected diseases. Amaranth is an azo dye which easily cleaved into amines and is suspected to be mutagen and carcinogen. Thus, the quantification of amaranth through reliable and sensitive sensor is of great importance. The SnO2/rGO nanocomposite has been engineered to be utilized as chemically modified sensor for the low-level quantification of amaranth in soft drinks and water sample. The fabricated nanocomposite materials was characterized through XRD, FTIR, raman and TEM tools which revealed average crystalline size of 23.7 nm, different surface functionalities and internal rectangle shaped morphology. The engineered nanocomposite was electrochemically characterized through electrochemical impedance spectroscopy (EIS) and Tafel plot to evaluate the electrocatalytic properties and charger transfer kinetics of SnO2/rGO/Nafion/GCE. The resistance of bare, GO/GCE and SnO2/rGO/Nafion/GCE was calculated as 812.5 Ω, 1343 Ω and 338 Ω. Certain parameters were optimized such as PBS electrolyte pH 6, scan rate 130 mV/s and potential window (0.4-1.2 V) to carry out sensitive and fluent determination process of amaranth azo dye. For the effectiveness of proposed sensor two calibration ranges were optimized from 1 to 800 nM and 1-60 µM. The LOD for both ranges were calculated as 0.68 nM and 0.0027 µM. Moreover, the anti-interference and stability profile of developed sensor were found phenomenal that suggest the exceptional electrocatalytic performance of SnO2/rGO/Nafion/GCE for amaranth.

Fabrication of sensor based on polyvinyl alcohol functionalized tungsten oxide/reduced graphene oxide nanocomposite for electrochemical monitoring of 4-aminophenol.

4-aminophenol (4-AP) is one of the major environmental pollutants which is broadly exploited as drug intermediate in the pharmaceutical formulations. The extensive release of 4-AP in the environment without treatment has become a serious issue that has led several health effects on humans. This work describe the determination of 4-AP through a new chemically modified sensor based on polyvinyl alcohol functionalized tungsten oxide/reduced graphene oxide (PVA/WO3/rGO) nanocomposite. The fabricated nanocomposite was characterized through XRD and HR-TEM to confirm the crystalline structure with average size of 35.9 nm and 2D texture with ultra-fine sheets. The electrochemical characterization of fabricated sensor was carried out by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) to ensure the charge transfer kinetics of modified sensor that revealed high conductivity of PVA/WO3/rGO/GCE. Under optimized conditions e.g. scan rate 80 mV/s, phosphate buffer (pH 6) as supporting electrolyte and potential window from -0.2 to 0.8 V, the prepared sensor showed excellent response for 4-AP. The linear dynamic range of developed method was optimized as 0.003-70 µM. The LOD of fabricated sensor based on PVA/WO3/rGO/GCE for 4-AP was calculated as 0.51 nM. The practical application of PVA/WO3/rGO/GCE was tested in real water and pharmaceutical samples. The fabricated sensor presented here, exhibited exceptional stability and sensitivity than the reported sensors and could be effectively used for the monitoring 4-AP without interferences.

Electrochemical quantification of mancozeb through tungsten oxide/reduced graphene oxide nanocomposite: A potential method for environmental remediation.

The extensive use of pesticides for better yield of crops have become major human concern over the decades. Pesticides are widely used in the fields to kill weeds and pests on the vegetable and crops to improve the quality and yield of the food knowing the fact that pesticides residue in food are very lethal for human being. Amongst, the hazardous pesticides, mancozeb is widely applied in the protection of crops. Thus the quantification of mancozeb residue is of great importance. This study reports the electrochemical monitoring of mancozeb through tungsten oxide reduced graphene oxide (WO3/rGO) nanocomposite. The engineered nanocomposite was characterized though different analytical tools such as FTIR, XRD and TEM to examine crystallinity, internal texture and the size. The FTIR result confirm the functionalities of GO and WO3/rGO nanocomposite in finger print and functional group region. Through XRD analysis, the size of the WO3/rGO nanocomposite was calculated as 31.6 nm. While the TEM analysis was also exploited to examine the 2D texture of GO and nanometric size of the WO3/rGO. To ensure the conductive nature of the WO3/rGO nanocomposite, the glassy carbon electrode was modified and exploited for cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Under the optimal conditions, the modified sensor showed exceptional response for mancozeb. The linear dynamic range was set from 0.05 to 70 µM in BRB buffer of pH 4. The LOD and LOQ for proposed method was calculated as 0.0038 and 0.0115 µM. The analytical applicability of chemically modified sensor was investigated in real matrix of different vegetable samples and the recovery values were observed in acceptable range. The electrochemical examination of present work reveals that WO3/rGO nanocomposite can be an exceptional aspirant for the determination of mancozeb at commercial level.

Spatial analysis and human health risk assessment of elements in ground water of District Hyderabad, Pakistan using ArcGIS and multivariate statistical analysis.

Availability of clean drinking water is a basic necessity of human population. Therefore, the current study was taken up for spatial analysis and human health risk assessment of elements in Ground water of District Hyderabad, Pakistan. Evaluation of 10 potential hazardous elements in one hundred eighteen samples of ground water from district Hyderabad, Pakistan was done to assess their natural and anthropogenic origin and possible effects on living organisms and human health. Based on statistical tools of Pearson Co-relation, Metal Clustering and Principal Component Analysis (PCA), three groups of elements were produced; First group included Mn, Fe, B and Cr, the second group contained Cu, Ni and As while third group included Pb, Cd and Zn. Higher Relative Standard Deviation (RSD) values of Cu, Ni, As, Pb, Cd and Zn showed their anthropogenic origin while Mn, Fe, B and Cr were found with lower concentration that indicated their natural origin. Histograms and box-plots of Mn, Fe, B and Cr were found to be normally distributed while these parameters were appeared abnormal for Cu, Ni, As, Pb, Cd and Zn. Risk assessment was quantified by hazard quotient (HQ) and cancer risk for both adult and child. Non-carcinogenic risks as depicted by HQs of all the 10 metal(loid)s were below the recommended HQ threshold of 1 for both child and adult. However, highest HQ was calculated for B (child 0.300 and adult 0.338) followed by the values for Mn and Ni. The potential risks of combined effect of all the 10 metal(loid)s through ingestion of groundwater was assessed using HI and calculated to be 0.694 for adult and 0.566 for child. This indicates the potential health risk of these metal(loid)s to human due to the consumption of the groundwater of district Hyderabad for drinking purpose. Considering the geometric mean for the studied area, carcinogenic risk of As through oral intake was calculated i.e. 1.50 × 10-4 and 2.62 × 10-5 for the adult and child However, this carcinogenic risk is 1.91 × 10-5 and 3.28 × 10-6 for Cd in adult and child and 1.94 × 10-3 and 3.32 × 10-4 for Cr in adult and child, respectively. Since the cancer risk 6exceeded the target risk of 1 × 10-4 for Cr i.e. 1.94 × 10-3 in adult, it can thus be considered as 'non-acceptable'. Spatial maps of elements produced by ArcGIS showed the hotspots of potential hazardous elements such as highest concentration of elements like Zn, Pb and Cd was found in urban areas while highest concentration of Cu, Ni and As was observed near Phulleli canal which passes from Hyderabad City and may contain contamination from waste material of residential area due to their anthropogenic activities.

Chemically Coupled Cobalt Oxide Nanosheets Decorated onto the Surface of Multiwall Carbon Nanotubes for Favorable Oxygen Evolution Reaction.

Cobalt oxide has been widely investigated among potential transition metal oxides for the electrochemical energy conversion, storage, and water splitting. However, they have inherently low electronic conductivity and high corrosive nature in alkaline media. Herein, we propose a promising and facile approach to improve the conductivity and charge transport of cobalt oxide Co3O4 through chemical coupling with well-dispersed multiwall carbon nanotubes (MWCNTs) during hydrothermal treatment. The morphology of prepared composite material consisting of nanosheets which are anchored on the MWCNTs as confirmed by scanning electron microscopy (SEM). A cubic crystalline system is exhibited by the cobalt oxide as confirmed by the X-ray diffraction study. The Co, O, and C are the only elements present in the composite material. FTIR study has indicated the successful coupling of cobalt oxide with MWCNTs. The chemically coupled cobalt oxide onto the surface of MWCNTs composite is found highly active towards oxygen evolution reaction (OER) with a low onset potential 1.44 V versus RHE, low overpotential 262 mV at 10 mAcm-2 and small Tafel slope 81 mV dec-1. For continuous operation of 40 hours during durability test, no decay in activity was recorded. Electrochemical impedance study further revealed a low charge transfer resistance of 70.64 Ohms for the composite material during the electrochemical reaction and which strongly favored OER kinetics. This work provides a simple, low cost, and smartly designing electrocatalysts via hydrothermal reaction for the catalysis and energy storage applications.

An advanced and efficient Co3O4/C nanocomposite for the oxygen evolution reaction in alkaline media.

The design of efficient nonprecious catalysts for the hydrogen evolution reaction (HER) or the oxygen evolution reaction (OER) is a necessary, but very challenging task to uplift the water-based economy. In this study, we developed a facile approach to produce porous carbon from the dehydration of sucrose and use it for the preparation of nanocomposites with cobalt oxide (Co3O4). The nanocomposites were studied by the powder X-ray diffraction and scanning electron microscopy techniques, and they exhibited the cubic phase of cobalt oxide and porous structure of carbon. The nanocomposites showed significant OER activity in alkaline media, and the current densities of 10 and 20 mA cm-2 could be obtained at 1.49 and 1.51 V versus reversible hydrogen electrode (RHE), respectively. The impedance study confirms favorable OER activity on the surface of the prepared nanocomposites. The nanocomposite is cost-effective and can be capitalized in various energy storage technologies.

Synthesis of Heart/Dumbbell-Like CuO Functional Nanostructures for the Development of Uric Acid Biosensor.

It is always demanded to prepare a nanostructured material with prominent functional properties for the development of a new generation of devices. This study is focused on the synthesis of heart/dumbbell-like CuO nanostructures using a low-temperature aqueous chemical growth method with vitamin B12 as a soft template and growth directing agent. CuO nanostructures are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) techniques. CuO nanostructures are heart/dumbbell like in shape, exhibit high crystalline quality as demonstrated by XRD, and have no impurity as confirmed by XPS. Apparently, CuO material seems to be porous in structure, which can easily carry large amount of enzyme molecules, thus enhanced performance is shown for the determination of uric acid. The working linear range of the biosensor is 0.001 mM to 10 mM with a detection limit of 0.0005 mM and a sensitivity of 61.88 mV/decade. The presented uric acid biosensor is highly stable, repeatable, and reproducible. The analytical practicality of the proposed uric acid biosensor is also monitored. The fabrication methodology is inexpensive, simple, and scalable, which ensures the capitalization of the developed uric acid biosensor for commercialization. Also, CuO material can be used for various applications such as solar cells, lithium ion batteries, and supercapacitors.

Quantitative separation of hesperidin, chrysin, epicatechin, epigallocatechin gallate, and morin using ionic liquid as a buffer additive in capillary electrophoresis.

Recently, an increasing interest has been observed in ionic liquids (ILs) due to their potentialities in various chemical processes. ILs have some unique properties making them excellent additives in CE. In this work a simple, rapid, and reliable CZE method has been developed and validated using 1-butyl-3-methyl imidazolium hexafluorophosphate (BMIM-PF6 ) ionic liquid as a buffer additive for the determination/separation of five flavonoids including hesperedin, epicatechin (EC), epigallocatechin gallate (EGCG), and morin using photodiode array (PDA) detector. The effect of several parameters such as concentration and pH of the running buffer, applied voltage, and concentration of ionic liquid were optimized. CZE at 25°C with 25 mM borate buffer of pH 9.0 at an applied voltage of 17 kV by adding 17.5 mM of IL was found to be suitable for the separation/determination of all five analytes within 08 min. Validation of the method was performed in terms of linearity, accuracy, precision, and limit of detection and quantification. The calibration curves were plotted in the concentration range of 1-200 µg/mL for all five analytes. The response was linear with R2  = 0.990 for EC, chrysin, and hesperidin, 0.992 for morin, and 0.988 for EGCG. LOD and LOQ were obtained within the range of 0.4-0.5 and 1.4-1.7 µg/mL, respectively. The proposed method showed good reproducibility with RSD of less than 3% for both migration time and peak height. The method was successfully applied for the determination of flavonoids from citrus fruits and tea samples.

A Robust, Enzyme-Free Glucose Sensor Based on Lysine-Assisted CuO Nanostructures.

The production of a nanomaterial with enhanced and desirable electrocatalytic properties is of prime importance, and the commercialization of devices containing these materials is a challenging task. In this study, unique cupric oxide (CuO) nanostructures were synthesized using lysine as a soft template for the evolution of morphology via a rapid and boiled hydrothermal method. The morphology and structure of the synthesized CuO nanomaterial were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The prepared CuO nanostructures showed high potential for use in the electrocatalytic oxidation of glucose in an alkaline medium. The proposed enzyme-free glucose sensor demonstrated a robust response to glucose with a wide linear range and high sensitivity, selectivity, stability, and reproducibility. To explore its practical feasibility, the glucose content of serum samples was successfully determined using the enzyme-free sensor. An analytical recovery method was used to measure the actual glucose from the serum samples, and the results were satisfactory. Moreover, the presented glucose sensor has high chemical stability and can be reused for repetitive measurements. This study introduces an enzyme-free glucose sensor as an alternative tool for clinical glucose quantification.

A novel micellar electrokinetic chromatographic method for separation of metal-DDTC complexes.

Micellar electrokinetic chromatography (MEKC) was examined for the separation and determination of Mo(VI), Cr(VI), Ni(II), Pd(II), and Co(III) as diethyl dithiocarbamate (DDTC) chelates. The separation was achieved from fused silica capillary (52 cm × 75 µm id) with effective length 40 cm, background electrolyte (BGE) borate buffer pH 9.1 (25 mM), CTAB 30% (100 mM), and 1% butanol in methanol (70 : 30 : 5 v/v/v) with applied voltage of -10 kV using reverse polarity. The photodiode array detection was achieved at 225 nm. The linear calibration for each of the element was obtained within 0.16-10 µg/mL with a limit of detection (LOD) 0.005-0.0167 µg/mL. The separation and determination was repeatable with relative standard deviation (RSD) within 2.4-3.3% (n = 4) in terms of migration time and peak height/peak area. The method was applied for the determination of Mo(VI) from potatoes and almond, Ni(II) from hydrogenated vegetable oil, and Co(III) from pharmaceutical preparations with RSD within 3.9%. The results obtained were checked by standard addition and rechecked by atomic absorption spectrometry.

Development and implication of a capillary electrophoresis methodology for ciprofloxacin, paracetamol and diclofenac sodium in pharmaceutical formulations and simultaneously in human urine samples.

This work studies the development of a simple and fairly rapid methodology for simultaneous determination/separation of three frequently co-administered drugs; ciprofloxacin (CIP), paracetamol (PCT) and diclofenac sodium (DIC) using capillary electrophoresis (CE) with UV detection at 260 nm. Separation was achieved in only 6.5 min with a simple buffer of sodium tetraborate (50 mM) at pH 9.0. The Parameters affecting the separation and detection were optimized. The calibration curves were linear in the range of 5-500 µg/mL for CIP, 5-250 µg/mL for PCT and 1-125 µg/mL for DIC sodium under the optimized conditions. The lower limit of detection (LOD) was found to be 1 µg/mL for CIP & PCT and 0.5 µg/mL for DIC. The method was successfully used for the analysis of drugs in commercial pharmaceutical formulations and simultaneously from patient's urine sample with RSD 0.5-2.4%. Results obtained with CE method are compared with standard HPLC procedure and were found in good agreement.

A capillary zone electrophoretic method for simultaneous determination of seven drugs in pharmaceuticals and in human urine.

A simple, sensitive, and novel method has been developed and validated for the separation and simultaneous quantitation of seven structurally different drugs-pipemidic acid and ofloxacin quinolone antibiotics, pseudoephedrine decongestant, piroxicam anti-inflammatory, thiamin, pyridoxine, and cobalamin-in a mixture by capillary zone electrophoresis. Factors affecting the separation were pH, concentration of buffer, and applied voltage. Separation was carried out in < 9 min with a 50 mM sodium tetraborate buffer, pH 10, and an applied voltage of 30 kV in an uncoated silica capillary tube. The carrier electrolyte gave baseline separation with good resolution, reproducibility, and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, and the lower LODs were within the range of 1-5 microg/mL. Detection was performed by UV absorbance at 230 nm. The method was validated for the analysis of drugs in pharmaceutical preparations and in urine samples with RSD of 0.5-2.4% and recovery of > 99%.

Quantitative separation of oxytocin, norfloxacin and diclofenac sodium in milk samples using capillary electrophoresis.

A simple, sensitive and rapid method has been developed for simultaneous separation and quantification of three different drugs: oxytocin (OT), norfloxacin (NOR) and diclofenac (DIC) sodium in milk samples using capillary electrophoresis (CE) with UV detection at 220 nm. Factors affecting the separation were pH, concentration of buffer and applied voltage. Separation was obtained in less than 9 min with sodium tetraborate buffer of pH 10.0 and applied voltage 30 kV. The separation was carried out from uncoated fused silica capillary with effective length of 50 cm with 75 microm i.d. The carrier electrolyte gave reproducible separation with calibration plots linear over 0.15-4.0 microg/mL for OT, 5-1000 microg/mL for NOR and 3-125 microg/mL for DIC. The lower limits of detection (LOD) were found to be 50 ng/mL for OT, and 1 microg/mL for NOR and DIC. The method was validated for the analysis of drugs in milk samples and pharmaceutical preparations with recovery of drugs within the range 96-100% with RSD 0.9-2.8%.