One-pot access to new tetrahydrobenzo[a]xanthen-11-ones and naphthopyranopyrimidines using 2,3-dihydroxynaphthalene

A one-pot, three-component reaction of 2,3-dihydroxynaphthalene, aromatic aldehydes, and cyclic 1,3-dicarbonyl compounds in the presence of formic acid catalyst under solvent-free conditions provides access toward a new class of tetrahydrobenzo[a]xanthen-11-ones and naphthopyranopyrimidines. The scope of the process was explored under two different reaction conditions resulting in the generation of title compounds in high yields. Moreover, the key advantages of this process are cost effectiveness of catalyst, short reaction times, easy workup, and purification of products by nonchromatographic methods.     

Development of a Reversed-Phase Liquid Chromatographic Assay for the Quantification of Total Persipeptides in Fermentation Broth

The emergence and prevalence of multi-drug-resistant bacterial strains increase the potential for outbreaks of incurable infections. The discovery of novel antibiotics and pharmacological preparations requires the identification of novel bioactive small molecules. A specific, sensitive, and reliable quantification method using high-performance liquid chromatography (HPLC) with UV detection was developed for the determination of total persipeptides (A and B), which are cyclic pentapeptides found in the fermentation broth of Streptomyces zagrosensis UTMC 1154 that exhibit bioactivity against methicillin-resistant Staphylococcus aureus (MRSA). A simple liquid–liquid extraction (LLE) method using butanol was employed to extract persipeptides from the fermentation broth prior to HPLC analysis. The chromatographic separation of persipeptides and the internal standard, virginiamycin, was achieved with a gradient of acetonitrile and water on a C18 reversed-phase analytical column in a 25-min analytical run utilizing a flow rate of 0.8 mL min⁻¹ and detection at 210 nm. The whole assay was validated, and the method presented a linear response range with a regression coefficient of determination R ² of 0.9996 for the quantification of persipeptides in the concentration range of 3.9–250.0 µg mL⁻¹, as well as extraction recoveries ranging from 54.78 ± 9.83 % to 56.45 ± 16.33 %. The bias and the precision of the proposed method were <10 %. The detection and quantification limits for the persipeptides were 27 and 83 µg L⁻¹, respectively.

     

Towards metals analysis using corona discharge ionization ion mobility spectrometry

For the first time, the capability of corona discharge ionization ion mobility spectrometry (CD-IMS) in the determination of metal complex was evaluated. The extreme simplicity of dispersive liquid–liquid microextraction (DLLME) coupled to the high sensitivity of CD-IMS measurement could make this combination really useful for simple, rapid, and sensitive determination of metals in different samples. In this regard, mercury, as a model metal, was complexed with diethyldithiocarbamate (DEDTC), and then extracted into the carbon tetrachloride using DLLME. Some parameters affecting the extraction efficiency, including the type and volume of the extraction solvent, the type and volume of the disperser solvent, the concentration of the chelating agent, salt addition and, pH were exhaustively investigated. Under the optimized condition, the enrichment factor was obtained to be 142. The linear range of 0.035–10.0 μg mL⁻¹ with r² = 0.997 and the detection limit of 0.010 μg mL⁻¹ were obtained. The relative standard deviation values were calculated to be lower than 4% and 8% for intra-day and inter-day, respectively. Finally, the developed method was successfully applied for the extraction and determination of mercury in various real samples. The satisfactory results revealed the capability of the proposed method in trace analysis without tedious derivatization or hydride generation.     

Facile Synthesis of Some Novel Tetrasubstituted 2,4‐Diaminopyrimidine Derivatives in Aqueous Glucose Solution as a Fully Green Medium and Promoter

A novel environmentally benign method toward the synthesis of some novel tetrasubstituted 2,4‐diaminopyrimidine derivatives using an aqueous glucose‐mediated one‐pot three‐component reaction of malononitrile with various benzaldehyde and amidine derivatives is reported. Some pyrimidine derivatives possessing α‐amino acid moiety were synthesized by the present protocol for the first time. This protocol offers advantages including facile reaction conditions, using naturally occurring glucose as promoter and water as solvent, simple work‐up, relatively short reaction times, and high yields of the products.     

Improved Photodegradation of Organic Contaminants Using Nano‐TiO2 and TiO2–SiO2 Deposited on Portland Cement Concrete Blocks

The photocatalytic activity of TiO₂ nanoparticles (nano‐TiO₂) and its hybrid with SiO₂ (nano‐TiO₂–SiO₂) for degradation of some organic dyes on cementitious materials was studied in this work. Nanohybrid photocatalysts were prepared using an inorganic sol–gel precursor and then characterized using XRD, SEM and UV–Vis. The grain sizes were estimated by Scherrer's equation to be around 10 nm. Then, a thin layer was applied to Portland cement concrete (PCC) blocks by dipping them into nano‐TiO₂ and nano‐TiO₂–SiO₂ solution. The efficiency of coated PCC blocks for the photocatalytic decomposition of two dyes, Malachite Green oxalate (MG) and Methylene Blue (MB), was examined under UV and visible irradiation and then monitored by the chemical oxygen demand tests. The results showed that more than 80% and 92% of MG and MB were decomposed under UV–Vis irradiation using blocks coated with nano‐TiO₂–SiO₂. TiO₂/PCC and TiO₂–SiO₂/PCC blocks showed a significant ability to oxidize dyes under visible and UV lights and TiO₂–SiO₂/PCC blocks require less time for dye degradation. Based on these results, coated blocks have increased photocatalytic activity which can make them commercially accessible photocatalysts.     

Application of phosphotungstic acid–nickel composite-modified carbon paste electrode for electrocatalytic oxidation of methanol in alkaline solution

Phosphotungstic acid (PWA) was used for accumulation of nickel ions at the carbon paste electrode for preparation of PWA-modified CPE (PWA/CPE). The PWA was evenly mixed with graphite powder and paraffin oil. Then, for preparation of Ni/PWA/CPE, Ni ions were included onto the PWA/CPE surface through immersion method at open circuit condition. The scanning electron microscopy (SEM), energy-dispersive spectroscopy and electrochemical methods were used to verify the prepared electrodes. The SEM images reveal that morphology of the CPE was influenced by PWA addition. Application of the Ni/PWA/CPE for methanol oxidation was explored by various electrochemical techniques. Electrochemical response of methanol oxidation at the surface of Ni/PWA/CPE was 2.5 times higher than that Ni/CPE. The obtained results indicated that the modified electrode exhibited high electrocatalytic activity toward methanol oxidation. Then, catalytic rate constant was found to be 8.25 × 10⁴ cm³ mol ^?1 s^?1 using chronoamperometry method. Furthermore, the effects of several parameters, such as PWA loading, NiSO₄ concentration, accumulation time and methanol concentration toward methanol oxidation at the surface of this modified electrode as well as stability, have been investigated.     

Resource allocation with stochastic optimal control approach

A control-theoretic decision making system is proposed for an agent (decision maker) to “optimally” allocate and deploy his/her resources over time among a dynamically changing list of opportunities (e.g., financial assets), in an uncertain market environment. The solution is a sequence of actions with the objective of optimizing total reward function. This control-theoretic approach is unique in a sense that it solves the problem at distinct time epochs over a finite time horizon and strategies are discovered directly. Rather than basing a decision making system on forecasts or training via a reinforcement learning algorithm using current state data, we train our system via a Q-learning algorithm using Geometric Brownian Motion as an asset price function. While the above problem is quite general, we focus solely on the problem of dynamic financial portfolio management with the objective of maximizing the expected utility for a given risk level. The performance functions that we consider for our system are realized mean return, drawdown and standard deviation. We find that our model achieves a better return and drawdown compared to a known market index as a benchmark.     

Sensitive Electrochemical Prostate Specific Antigen Aptasensor: Effect of Carboxylic Acid Functionalized Carbon Nanotube and Glutaraldehyde Linker

The performance of carboxylic acid functionalized carbon nanotubes (CNTs_(COOH)), chitosan (Chit), carbon nanotubes‐chitosan (CNTs‐Chit and CNTs_(COOH)‐Chit) for immobilizing of amino‐functionalized ssDNA and fabrication of electrochemical prostate specific antigen (PSA) aptasensor were studied in detail using X‐ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT‐IR) and electrochemical impedance spectroscopy (EIS). The assemblies of capture probe are formed on the surface via two approaches: EDC/NHS chemistry and glutaraldehyde linker. Cyclic voltammetry (CV), differential pulse voltammetry (DPV) and EIS techniques were used to investigate the analytical performance of the PSA aptasensor. Under optimum conditions the sensitivity of 0.0026 µA/(ng/ml) and a limit of detection of 0.75 ng/ml (22 pM) were obtained for PSA detection. This protocol offers a new means for sensitive detection of PSA with some advantages in terms of simplicity, selectivity, ease of use and regenerability.