Electrocatalytic oxidation of salicylic acid at a carbon paste electrode impregnated with cerium-doped zirconium oxide nanoparticles as a new sensing approach for salicylic acid determination

Cerium-doped zirconium oxide (Ce/ZrO₂) was introduced as a highly efficient electrocatalyst for electrooxidation of salicylic acid (SA). The electrocatalyst material was synthesized via co-precipitation of cerium and zirconium ions, and then the resulting solid was heat-treated at high temperature to create crystallized cerium-doped zirconium oxide nanoparticles. The obtained material was characterized by scanning electron microscopy and X-ray diffraction methods. The Ce/ZrO₂-modified carbon paste electrode (Ce/ZrO₂-CPE) exhibited a distinct oxidative peak for SA, whereas no signal was observed for SA at unmodified carbon paste electrode at the same experimental conditions. Cyclic voltammetry and electrochemical impedance spectroscopy were applied to investigate the electrocatalytic performance of the electrode and SA electrooxidation mechanism. Square wave voltammetry was used to capture the analytical signal of SA. The electrode composition was optimized to increase the SA signal. Using the optimized electrode, it became possible to determine SA in the concentration range of 5.0–1000.0 μM with detection limit of 1.1 μM (3S_b/m). The electrode showed very high sensitivity of 1013.5 μA mM^?1 cm^?2 which is remarkably better than the previously reported SA sensors. The proposed method was successfully applied for the determination of SA in human serum, milk, and pharmaceutical samples.     

Rapid micellar HPLC analysis of loratadine and its major metabolite desloratadine in nano-concentration range using monolithic column and fluorometric detection: application to pharmaceuticals and biological fluids

Background

Loratadine is a commonly used selective non-sedating antihistaminic drug. Desloratadine is the active metabolite of loratadine and, in addition, a potential impurity in loratadine bulk powder stated by the United States Pharmacopeia as a related substance of loratadine. Published methods for the determination of both analytes suffer from limited throughput due to the time-consuming steps and tedious extraction procedures needed for the analysis of biological samples. Therefore, there is a strong demand to develop a simple rapid and sensitive analytical method that can detect and quantitate both analytes in pharmaceutical preparations and biological fluids without prior sample extraction steps.

Results

A highly-sensitive and time-saving micellar liquid chromatographic method is developed for the simultaneous determination of loratadine and desloratadine. The proposed method is the first analytical method for the determination of this mixture using a monolithic column with a mobile phase composed of 0.15 M sodium dodecyl sulfate, 10% n-Butanol and 0.3% triethylamine in 0.02 M phosphoric acid, adjusted to pH 3.5 and pumped at a flow rate of 1.2 mL/min. The eluted analytes are monitored with fluorescence detection at 440 nm after excitation at 280 nm. The developed method is linear over the concentration range of 20.0–200.0 ng/mL for both analytes. The method detection limits are 15.0 and 13.0 ng/mL and the limits of quantification are 20.0 and 18.0 ng/mL for loratadine and desloratadine, respectively. Validation of the developed method reveals an accuracy of higher than 97% and intra- and inter-day precisions with relative standard deviations not exceeding 2%.

Conclusions

The method can be successfully applied to the determination of both analytes in various matrices including pharmaceutical preparations, human urine, plasma and breast milk samples with a run-time of less than 5 min and without prior extraction procedures. The method is ideally suited for use in quality control laboratories. Moreover, it could be a simple time-saving alternative to the official pharmacopeial method for testing desloratadine as a potential impurity in loratadine bulk powder.

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Graphical abstract Typical chromatogram of loratadine and its major metabolite desloratadine using the proposed micellar HPLC method

     

Phytochemistry,Food Application,and Therapeutic Potential of the Medicinal Plant (Withania coagulans): A Review

Herbal plants have been utilized to treat and cure various health-related problems since ancient times. The use of Ayurvedic medicine is very significant because of its least reported side effects and host of advantages. Withania coagulans (Family; Solanaceae), a valuable medicinal plant, has been used to cure abnormal cell growth, wasting disorders, neural as well as physical problems, diabetes mellitus, insomnia, acute and chronic hepatic ailments. This review provides critical insight regarding the phytochemistry, biological activities, and pharmacognostic properties of W. coagulans. It has been known to possess diuretic, anti-inflammatory, anti-bacterial, anti-fungal, cardio-protective, hepato-protective, hypoglycemic, anti-oxidative, and anti-mutagenic properties owing to the existence of withanolides, an active compound present in it. Apart from withanolides, W. coagulans also contains many phytochemicals such as flavonoids, tannins, and β-sterols. Several studies indicate that various parts of W. coagulans and their active constituents have numerous pharmacological and therapeutic properties and thus can be considered as a new drug therapy against multiple diseases.     

An Intricate Review on Nutritional and Analytical Profiling of Coconut,Flaxseed, Olive,and Sunflower Oil Blends

Vegetable oils (VOs), being our major dietary fat source, play a vital role in nourishment. Different VOs have highly contrasting fatty acid (FA) profiles and hence possess varying levels of health protectiveness. Consumption of a single VO cannot meet the recommended allowances of various FA either from saturated FA (SFA), monounsaturated FA (MUFA), polyunsaturated FA (PUFA), Ω-3 PUFAs, and medium-chain triglycerides (MCTs). Coconut oil (CO), flaxseed oil (FO), olive oil (OO), and sunflower oil (SFO) are among the top listed contrast VOs that are highly appreciated based on their rich contents of SFAs, Ω-3 PUFAs, MUFAs, and Ω-6 PUFA, respectively. Besides being protective against various disease biomarkers, these contrasting VOs are still inappropriate when consumed alone in 100% of daily fat recommendations. This review compiles the available data on blending of such contrasting VOs into single tailored blended oil (BO) with suitable FA composition to meet the recommended levels of SFA, MUFA, PUFA, MCTs, and Ω-3 to Ω-6 PUFA ratios which could ultimately serve as a cost-effective dietary intervention towards the health protectiveness and improvement of the whole population in general. The blending of any two or more VOs from CO, FO, OO, and SFO in the form of binary, ternary, or another type of blending was found to be very conclusive towards balancing FA composition; enhancing physiochemical and stability properties; and promising the therapeutic protectiveness of the resultant BOs.     

Improved visible light photocatalytic activity of TiO<Subscript>2</Subscript> nano powders with metal ions doping for glazed ceramic tiles

Self-cleaning and anti-bacterial activities of the photo-catalyst titanium dioxide make it a superior compound for use in the ceramics and glass industry. In order to achieve high self-cleaning efficiency for building products, it is important that Titania is present as anatase phase. Moreover, it is desirable that the particle sizes are in Nano-range, so that a large enough surface area is available for enhanced catalytic performance. In the present paper, Cobalt and Nickel co-doped (4%mol Ni and 4%mol Co doped TiO₂) and un-doped TiO₂ Nano powders have been prepared by sol–gel technique. They were calcined at the temperatures in the range of 475–1075 °C. Ni/Co co-doped TiO₂ postponed the anatase to rutile transformation of TiO₂ by about 200–300°C, such that before calcination at 775°C, no rutile was detected for 4 mol% Ni/Co co-doped TiO₂. A systematic decreasing on crystallite size and increasing on specific surface area of Ni/Co co-doped TiO₂ were observed. Photo-catalytic activity of anatase polymorph was measured by the decomposition rate of methylene blue under visible light. The results showed enhanced catalysis under visible light for Ni/Co co-doped TiO₂ as compared to pure TiO₂. The enhanced performance was attributed to surface chemistry change associated with a slight shift in the band gap. Depending on the temperatures ranging from 475 to 1075 °C, band gap energy of Ni and Co doped TiO₂ crystals decreased. For all samples there is a general reduction of the band gap energy from 3.00 to 2.96 eV.     

Multiple Spectroscopic,Docking and Cytotoxic Study of a Synthesized 2,2′ Bipyridin Phenyl Isopentylglycin Pt(II) Nitrate Complex: Human Serum Albumin and Breast Cancer Cell Line of MDA-MB231 as Targets

In the present study, the biological activities of a new synthesized Pt(II)-complex, 2,2′ bipyridinphenyl isopentylglycin Pt(II) nitrate was investigated via its interaction with the most important blood carrier protein of human serum albumin (HSA), using fluorescence and Far-UV circular dichroism (CD) spectroscopic techniques and also molecular docking. Moreover, cytotoxicity activity of the complex was studied against breast cancer cell line of MDA MB231 using 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The Pt(II)-complex has a strong ability to quench the intrinsic fluorescence of HSA through a static quenching mechanism. According fluorescence quenching data, the binding parameters of the interaction were calculated and showed that hydrophobic interaction has an important role. The molecular docking results in coherent with fluorescence measurements illustrated that Pt(II) complex can bind to HSA at one position that located in the hydrophobic cavity of groove between drug site I and II. Also, experimental data on driving force in binding site was confirmed whereas theoretical results demonstrated Pt(II) complexinteract to HSA by hydrophobic interaction. Far-UV-CD results showed that Pt(II)-complex induced an increasing in the content of α-helical structure of the protein and stabilized it. Also, MTT assay represented growth inhibitory effect of the complex toward the breast cancer cell line.     

On the improvement of signal repeatability in laser-induced air plasmas

The relatively low repeatability of laser-induced breakdown spectroscopy (LIBS) severely hinders its wide commercialization. In the present work, we investigate the optimization of LIBS system for repeatability improvement for both signal generation (plasma evolution) and signal collection. Timeintegrated spectra and images were obtained under different laser energies and focal lengths to investigate the optimum configuration for stable plasmas and repeatable signals. Using our experimental setup, the optimum conditions were found to be a laser energy of 250 mJ and a focus length of 100 mm. A stable and homogeneous plasma with the largest hot core area in the optimum condition yielded the most stable LIBS signal. Time-resolved images showed that the rebounding processes through the air plasma evolution caused the relative standard deviation (RSD) to increase with laser energies of > 250 mJ. In addition, the emission collection was improved by using a concave spherical mirror. The line intensities doubled as their RSDs decreased by approximately 25%. When the signal generation and collection were optimized simultaneously, the pulse-to-pulse RSDs were reduced to approximately 3% for O(I), N(I), and H(I) lines, which are better than the RSDs reported for solid samples and showed great potential for LIBS quantitative analysis by gasifying the solid or liquid samples.     

Spin transfer torque in the semiconductor/ferromagnetic structure in the presence of Rashba effect

Spin transfer torque in magnetic structure occurs when the transverse component of the spin current that flows from the nonmagnetic medium to ferromagnetic medium is absorbed by the interface. In this paper, considering the Rashba effect on the semiconductor region, we discuss the spin transfer torque in semiconductor/ferromagnetic structure and obtain the components of spin-current density for two models:(i) single electron and(ii) the distribution of electrons. We show that no matter whether the difference in Fermi surface between semiconductor and Fermi spheres for the up and down spins in ferromagnetic increases, the transmission probability decreases. The obtained results for the values used in this article illustrate that Rashba effect increases the difference in Fermi sphere between semiconductor and Fermi sphere for the up and down spins in ferromagnetic. The results also show that the Rashba effect, brings an additional contribution to the components of spin transfer torque, which does not exist in the absence of the Rashba interaction. Moreover, the Rashba term has also different effects on the transverse components of the spin torque transfer.     

Comparative Study of the Synthetic Approaches and Biological Activities of the Bioisosteres of 1,3,4-Oxadiazoles and 1,3,4-Thiadiazoles over the Past Decade

The bioisosteres of 1,3,4-oxadiazoles and 1,3,4-thiadiazoles are well-known pharmacophores for many medicinally important drugs. Throughout the past 10 years, 1,3,4-oxa-/thiadiazole nuclei have been very attractive to researchers for drug design, synthesis, and the study of their potential activity towards a variety of diseases, including microbial and viral infections, cancer, diabetes, pain, and inflammation. This work is an up-to-date comparative study that identifies the differences between 1,3,4-thiadiazoles and 1,3,4-oxadiazoles concerning their methods of synthesis from different classes of starting compounds under various reaction conditions, as well as their biological activities and structure–activity relationship.