Simultaneous determination of trace amounts of anti-hypertensive drugs in urine using magnetic mixed hemimicelles solid-phase extraction combined with HPLC-UV

Hypertension is the leading cause of morbidity and mortality in developed and developing countries. The combination of amlodipine and carvedilol is very effective for reducing blood pressure and improving treatment compliance. Determination of drugs in biological fluids is vital in therapeutic efficacy. In the present study, a simple, rapid and efficient magnetic solid phase extraction procedure based on mixed hemimicelles is described and validated for the simultaneous determination of trace amounts of anti-hypertensive drugs in urine samples using sodium dodecyl sulfate-coated magnetite nanoparticles as extractant. Various factors, which could affect the extraction efficiency were investigated and optimized. Under the optimum conditions, the limits of detection (S/N = 3) for amlodipine and carvedilol were 5 and 2 ng/mL, respectively. The relative standard deviation for six measurements of 50 ng/mL of amlodipine and carvedilol were 4.7 and 5.2%, respectively. The developed method was applied to the analysis of patients' urine samples, and satisfactory results were obtained in the range between 81.6 and 92.7%.     

Turbulence control in wall-bounded flows by spanwise oscillations

The feasibility of control of wall turbulence by high frequency spanwise oscillations is investigated by direct numerical simulations of a planar turbulent channel flow subjected either to an oscillatory spanwise crossflow or to the spanwise oscillatory motion of one of the channel walls. Periods of oscillation,T _osc. ⁺ =T _osc. u ² /v, ranging from 25 to 500 were studied. For 25<T _osc. ⁺ <200 production of turbulence is suppressed. The most effective suppression of turbulence occurs atT _osc ⁺ =100, for which the overall turbulence production is reduced by 62% compared to the unperturbed channel and sustained turbulent drag reductions of 40% are obtained. The suppression of turbulence is due to a continual shift of the near wall streamwise vortices relative to the wall layer streaks, which in turn leads to a widening, merging and weakening of the wall layer streaks and an overall reduction in the turbulence production. The turbulence suppression mechanism observed in these studies opens up new possibilities for effective control of turbulence in wall-bounded flows.     

Synthesis, biological and computational study of new Schiff base hydrazones bearing 3-(4-pyridine)-5-mercapto-1,2,4-triazole moiety

A series of new Schiff base hydrazones (compounds 1-16) were synthesized by condensation reaction of 4-amino-3-(4-pyridine)-5-mercapto-1,2,4-triazole with various aldehydes and/or dialdehydes. The structure of the prepared compounds was confirmed by means of 1H NMR, 13C NMR, UV-vis, IR and elemental analyses. The all prepared compounds were assayed for antibacterial (Escherichia coli and Staphylococcus aureus) and antifungal (Candida albicans) activities by disc diffusion method. The results indicate that all tested compounds did not show any antibacterial activity against E. coli, as gram negative bacteria, and antifungal activity against C. albicans. But the compounds 2, 3, 4, 6 and 8 containing 4-Cl, 4-Me, 4-MeO, 2,4-di-Cl and 2-OH substituted phenyl moiety, respectively, showed good inhibition against S. aureus as compare to standard drugs. The structure of all biologically active compounds has also been theoretically studied by ab initio Hartree-Fock (HF) methods.     

Intramolecular hetero-Diels-Alder reaction of 1-oxa-1,3-butadienes with terminal acetylenes in aqueous media using CuI

A new method for the preparation of tetracyclic uracils (oxa-helicene) 4 was developed. The intramolecular hetero-Diels-Alder reaction of 1-oxa-1,3-butadiene 3 and an unactivated alkyne in the presence of CuI led to tetracyclic uracils 4 in aqueous media with good yields. The 1-oxa-1,3-butadiene 3 was prepared through Knoevenagel reaction of O-propargylated salicylaldehyde derivatives and barbituric acid or 1,3-dimethylbarbituric acid.     

Photo-Physical Behavior and Fluorescence of Thermo Switchable Nanocomposite Based on Methyl Methacrylate -Spirobenzopyran

Nanocomposites with thermo and photo-switchable fluorescent properties were synthesized via mini-emulsion polymerization based on spiropyran and methyl methacrylate monomer. The photophysical behavior of fluorescence nanocomposites was investigated by fluorescence spectrophotometry in different temperature, UV-light and time of exposure. It was found that methyl methacrylate polymer is capable of acting as a protective layer and play a critical role in improving the photostability of colorants. The nanocomposites exhibited excellent fluorescent thermo-switching action with respect to the free spiro molecule.

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One‐pot multicomponent synthesis of novel 2‐(piperazin‐1‐yl) quinoxaline and benzimidazole derivatives,using a novel sulfamic acid functionalized Fe3O4 MNPs as highly effective nanocatalyst

The immobilization of sulfonic acid on the surface of Fe₃O₄ magnetic nanoparticles (MNPs) as a novel acid nanocatalyst has been successfully reported. The morphological features, thermal stability, magnetic properties, and other physicochemical properties of the prepared superparamagnetic core–shell (Fe₃O₄@PFBA–Metformin@SO₃H) were thoroughly characterized using Fourier transform infrared (FTIR), X‐ray diffraction (XRD), energy‐dispersive X‐ray spectroscopy (EDS), field‐emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), thermogravimetric analysis–differential thermal analysis (TGA‐DTA), atomic force microscopy (AFM), dynamic light scattering (DLS), Brunauer–Emmett–Teller (BET), and vibrating sample magnetometer (VSM) techniques. It was applied as an efficient and reusable catalyst for the synthesis of 2‐(piperazin‐1‐yl) quinoxaline and benzimidazole derivatives via a one‐pot multiple‐component cascade reaction under green conditions. The results displayed the excellent catalytic activity of Fe₃O₄@PFBA–metformin@SO₃H as an organic–inorganic hybrid nanocatalyst in condensation and multicomponent Mannich‐type reactions. The easy separation, simple workup, excellent stability, and reusability of the nanocatalyst and quantitative yields of products and short reaction time are some outstanding advantages of this protocol.     

Remarkable Improvement of Methylglyoxal Synthase Thermostability by His–His Interaction

Lately it has been proposed that interaction between two positively charged side chains can stabilize the folded state of proteins. To further explore this point, we studied the effect of histidine–histidine interactions on thermostability of methylglyoxal synthase from Thermus sp. GH5 (TMGS). The crystal structure of TMGS revealed that His23, Arg22, and Phe19 are in close distance and form a surface loop. Here, two modified enzymes were produced by site-directed mutagenesis (SDM); one of them, one histidine (TMGS-HH^O), and another two histidines (TMGS-HHH^O) were inserted between Arg22 and His23 (H^O). In comparison with the wild type, TMGS-HH^O thermostability increased remarkably, whereas TMGS-HHH^O was very unstable. To explore the role of His23 in the observed phenomenon, the original His23 in TMGS-HHH^O was replaced with Ala (TMGS-HHA). Our data showed that the half-life of TMGS-HHA decreased in relation to the wild type. However, its half-life increased in comparison with TMGS-HHH^O. These results demonstrated that histidine–histidine interactions at position 23 in TMGS-HH^O probably have the main role in TMGS thermostability.     

热分解双(2-氨基烟酸)锌(Ⅱ)制备的介孔微砖ZnO纳米颗粒的光催化活性(英文)

Hollow microblocks of [Zn(anic)_2], as a novel coordination compound, were synthesized using 2-aminonicotinic acid(Hanic) and zinc(Ⅱ) nitrate tetrahydrate. The chemical composition of the zinc complex, ZnC_(12)H_(10)N_4O_4, was determined by Fourier transform infrared(FTIR) spectroscopy and elemental analysis. The synthesized zinc complex was used as a precursor to produce ZnO nanostructures by calcination at 550 °C for 4 h. Morphological studies by scanning electron microscopy and transmission electron microscopy revealed the formation of porous microbricks of ZnO nanoparticles. N_2 adsorption-desorption analysis showed that the obtained ZnO microbricks possess a mesoporous structure with a surface area of 8.13 m~2/g and a pore size of 22.6 nm. The X-ray diffraction pattern of the final product proved the formation of a pure ZnO composition with a hexagonal structure. Moreover, FTIR analyses showed that the 2-aminonicotinic acid ligand peaks were absent after the calcination step. Diffuse reflectance spectroscopy was used to determine the band gap energy of the produced ZnO and it was about 3.19 eV. To investigate the photocatalytic activity of the porous ZnO nanostructure, a series of photocatalytic tests were carried out to remove Congo red, as a representative toxic azo dye, from aqueous solution. The results show that the product can be used as an efficient photocatalyst for waste water treatment with high degradation efficiency.     

Derivations of Direct Limits of Lie Superalgebras

We describe the derivations of a direct limit 𝔏 of Lie superalgebras 𝔏ⁱ (i ∈ I) in an 𝔏-module 𝔲 as the inverse limit of the derivations of 𝔏ⁱ's in 𝔲. Using this, in case the first cohomology group of each 𝔏ⁱ with coefficients in 𝔲 is zero, we describe the derivations of 𝔏 in 𝔲 as the inverse limit of 𝔲/𝔲𝔏ⁱ (i ∈ I). This then allows us to compute the derivations of direct limits of finite-dimensional basic classical simple Lie superalgebras.