Selective back-extraction and preconcentration of zinc(II) from metal-1,3,5-triketone extracts prior to its determination by flame atomic absorption spectrometry

A simple back-extraction method was developed for the separation and preconcentration of trace levels of zinc from different matrices. Ethyl-2-(4-methoxybenzoyl)-3-(4-methoxyphenyl)-3-oxopropanoylcarbamate (EMPC) was used as a new complexing agent for the extraction of zinc(II) from the aqueous sample phase to the methyl isobutyl ketone (MIBK) phase as Zn(EMPC)₂ complexes. The Zn(II) can be selectively stripped with 1?mL of 0.5?mol?L^?1 HCl from Mⁿ⁺(EMPC)_n complexes [Ag(I), Al(III), Cd(II), Cr(III), Cu(II), Fe(II), Fe(III), Mn(II), Ni(II), Pb(II) and Pd(II)] which dissolved in MIBK phase. Some experimental parameters, which are important for the whole extraction process, including pH, sample volume, shaking time, amount of the EMPC reagent, amount of MIBK, ionic strength, and type of back-extractant were investigated. The recovery for Zn(II) was greater than 95%. The detection limit of the method was found to be 0.2?µg?L ^{? 1} and the relative standard deviation as 6.4%. The concentrations of Zn(II) in the certified reference materials (LGC6019 river water and NIST-1547 peach leaves) by the presented method were in good agreement with the certified values. The proposed method was succesfully applied to the determination of zinc in some natural waters, rice, hair, soil, and tea samples.     

Preparation of calix[4]arene-based sporopollenin and examination of its dichromate sorption ability

The present study describes the preparation of a new calix[4]arene-based sporopollenin material and its application for the removal of Na₂Cr₂O₇ from aqueous solution. The novel calix[4]arene-based sporopollenin material was prepared via the immobilization of dihydrazine amide derivative of p-tert-butylcalix[4]arene (3) onto the modified sporopollenin. The newly prepared calix[4]arene-based sporopollenin is characterized by using different analytical techniques such as FT-IR spectroscopy, scanning electron microscope and Elemental analysis. The batch wise sorption study was carried out to optimize various experimental parameters such as the effect of sorbent dosage, pH, temperature and Cr(VI) anion concentration. It has been found that the sorption of Cr(VI) anion on calix[4]arene-based sporopollenin was highly pH dependent and maximum sorption was achieved at pH 1.5. The sorption behavior was also evaluated by Langmuir, Freundlich and Dubinin Radushkevich isotherms. The value of correlation coefficient (R ²) showed a good agreement with Freundlich isotherm model. Result of study demonstrated that calix[4]arene-based sporopollenin proved to be highly effective for the removal of Cr(VI).     

Synthesis, characterization, and biological evaluation of new oxime-phosphazenes

Hexachlorocylotriphosphazene (1) was reacted with 4-hydroxy-3-methoxybenzaldehyde to give hexakis[(4-formyl-2-methoxy)phenoxy]cyclotriphosphazene (2). Hexakis[(4-(hydroxyimino)2-methoxy)phenoxy]cyclotriphosphazene (3) was synthesized by reaction of 2 with hydroxlamine hydrochloride in pyridine. Compound 3 was reacted with benzyl chloride, acetyl chloride, allyl bromide, benzoyl chloride, propanoyl chloride, 4-methoxybenzoyl chloride, 2-chlorobenzoyl chloride, chloroacetyl chloride, methyl iodide, and thiophene-2-carbonyl chloride. From these reactions, full or partially substituted compounds were obtained, usually in high yields. Pure or defined products could not be obtained from reaction of 3 with methacryloyl chloride and O-acetylsalicyloyl chloride. The structures of the compounds were determined by elemental analysis, and IR, ¹H, ¹³C, and ³¹P NMR spectroscopy. The synthesized compounds were screened for in-vitro antimicrobial activity against two Gram-positive bacteria (Staphylococcus aureus and Enterococcus faecalis), two gram-negative bacteria (Escherichia coli and Klebsiella pneumonia), and fungal strains (Aspergillus niger, and Candida albicans) by the agar well diffusion method. Few compounds had significant activity against both Gram-positive and Gram-negative bacteria. None of the compounds had antifungal activity except compounds 7 and 9, which had moderate activity.     

Brønsted acidic magnetic nano-Fe3O4-adorned calix[n]arene sulfonic acids: synthesis and application in the nucleophilic substitution of alcohols

Three magnetically recoverable Brønsted acidic calix[n]arene derivatives were successfully constructed by immobilizing calix[n]arene sulfonic acids onto silica-coated magnetic nanoparticles, a process, which allows calix[n]arene derivatives to acquire magnetic properties. All of the magnetically recoverable Brønsted acidic calix[n]arenes efficiently catalyze the coupling of electron-rich arenes with some alcohols in water. After separation and recovery from the reaction mixture by a simple magnet, these Brønsted acidic calix[n]arenes can be recycled many times without losing their catalytic activity.     

A flow-through microfluidic chip for continuous dielectrophoretic separation of viable and non-viable human T-cells

Effective methods for rapid sorting of cells according to their viability are critical in T cells based therapies to prevent any risk to patients. In this context, we present a novel microfluidic device that continuously separates viable and non-viable T-cells according to their dielectric properties. A dielectrophoresis (DEP) force is generated by an array of castellated microelectrodes embedded into a microfluidic channel with a single inlet and two outlets; cells subjected to positive DEP forces are drawn toward the electrodes array and leave from the top outlet, those subjected to negative DEP forces are repelled away from the electrodes and leave from the bottom outlet. Computational fluid dynamics is used to predict the device separation efficacy, according to the applied alternative current (AC) frequency, at which the cells move from/to a negative/positive DEP region and the ionic strength of the suspension medium. The model is used to support the design of the operational conditions, confirming a separation efficiency, in terms of purity, of 96% under an applied AC frequency of 1.5 × 10⁶ Hz and a flow rate of 20 μl/h. This work represents the first example of effective continuous sorting of viable and non-viable human T-cells in a single-inlet microfluidic chip, paving the way for lab-on-a-chip applications at the point of need.     

Synthesis of attapulgite-MnO2 nanocomposite from manganese complex by ultrasound for hydrogen storage

The research included the synthesis of a new complex of manganese with 3,4,5-tri-methoxybenzoic acid in the presence of triethylamine as a base to which gives the complex with formula [Mn (TMB)₂].2H₂O. This complex was characterized by FTIR, CHN, magnetic susceptibility and thermal analysis. Furthermore, this complex was used as a novel precursor of manganese in preparing the attapulgite-MnO₂ nanocomposite by one-pot addition method using ultrasound. The resulting nanocomposite was characterized by X-ray diffraction and TEM and the results prove that this composite was found as nanochannel of the diameter 45 nm decorated with 26–41 nm of MnO₂ nanoparticles. The attapulgite-MnO₂ nanocomposite was used in the application of hydrogen storage, and the results proved that attapulgite-MnO₂ nanocomposite has the ability to store 3.55 wt% of hydrogen under a pressure of 90 bar and a temperature of 77 K. Furthermore, the measurement demonstrated that increasing the pressure increased the stored hydrogen, implying that the stored gas will be liberated by altering the pressure, implying that the storage will be of the physical kind.     

Solubility and Stability of Some Pharmaceuticals in Natural Deep Eutectic Solvents-Based Formulations

Some medicines are poorly soluble in water. For tube feeding and parenteral administration, liquid formulations are required. The discovery of natural deep eutectic solvents (NADES) opened the way to potential applications for liquid drug formulations. NADES consists of a mixture of two or more simple natural products such as sugars, amino acids, organic acids, choline/betaine, and poly-alcohols in certain molar ratios. A series of NADES with a water content of 0–30% (w/w) was screened for the ability to solubilize (in a stable way) some poorly water-soluble pharmaceuticals at a concentration of 5 mg/mL. The results showed that NADES selectively dissolved the tested drugs. Some mixtures of choline-based NADES, acid-neutral or sugars-based NADES could dissolve chloral hydrate (dissociated in water), ranitidine·HCl (polymorphism), and methylphenidate (water insoluble), at a concentration of up to 250 mg/mL, the highest concentration tested. Whereas a mixture of lactic-acid–propyleneglycol could dissolve spironolacton and trimethoprim at a concentration up to 50 and 100 mg/mL, respectively. The results showed that NADES are promising solvents for formulation of poorly water-soluble medicines for the development of parenteral and tube feeding administration of non-water-soluble medicines. The chemical stability and bioavailability of these drug in NADES needs further studies.     

Polyethylene Glycol Functionalized Graphene Oxide Nanoparticles Loaded with Nigella sativa Extract: A Smart Antibacterial Therapeutic Drug Delivery System

Flaky graphene oxide (GO) nanoparticles (NPs) were synthesized using Hummer’s method and then capped with polyethylene glycol (PEG) by an esterification reaction, then loaded with Nigella sativa (N. sativa) seed extract. Aiming to investigate their potential use as a smart drug delivery system against Staphylococcus aureus and Escherichia coli, the spectral and structural characteristics of GO-PEG NPs were comprehensively analyzed by XRD, AFM, TEM, FTIR, and UV- Vis. XRD patterns revealed that GO-PEG had different crystalline structures and defects, as well as a higher interlayer spacing. AFM results showed GONPs with the main grain size of 24.41 nm, while GONPs–PEG revealed graphene oxide aggregation with the main grain size of 287.04 nm after loading N. sativa seed extract, which was verified by TEM examination. A strong OH bond appeared in FTIR spectra. Furthermore, UV- Vis absorbance peaks at (275, 284, 324, and 327) nm seemed to be correlated with GONPs, GO–PEG, N. sativa seed extract, and GO –PEG- N. sativa extract. The drug delivery system was observed to destroy the bacteria by permeating the bacterial nucleic acid and cytoplasmic membrane, resulting in the loss of cell wall integrity, nucleic acid damage, and increased cell-wall permeability.     

Host-guest molecular encapsulation of cucurbit[7]uril with dillapiole congeners using docking simulation and density functional theory approaches

Structural Chemistry - Binding affinity and intermolecular interactions are essential characteristics that could be used to comprehend molecular recognition between molecules in supramolecular...