Development and Validation Method for Silica Determination by Spectrophotometry in Some Herbs and Pharmaceutical Formulations

ABSTRACT

A spectrophotometric method for determination of silica in herbs and herbal pharmaceutical products has been developed and validated. The method showed excellent accuracy and precision with S.D. 1.67 and RSD 1.72%, 2.75%, respectively. The established linearity range was 0.05–0.5 μg/mL(r² > 0.99974). The recovery of silica from spiked placebo was > 95% over the linear range. The method has been successfully used in the analysis of silica in raw material and herbal pharmaceutical formulations. This validated method proved to be rapid and less costly.     

Silica gel-mediated hydrohalogenation of unactivated alkenes using hydrohalogenic acids under organic solvent-free conditions

Silica gel-mediated hydrochlorination of unactivated alkenes using 35% hydrochloric acid under organic solvent-free conditions proceeded to give the corresponding chlorides in good yields. Hydrobromination or hydriodination using 47% hydrobromic acid or 55% hydriodic acid afforded the corresponding halides, respectively. Silica gel could be recycled five times without any significant loss of activities.     

Metal Oxide Assisted Preparation of Core–Shell Beads with Dense Metal–Organic Framework Coatings for the Enhanced Extraction of Organic Pollutants

Dense and homogeneous metal–organic framework (MOF) coatings on functional bead surfaces are easily prepared by using intermediate sacrificial metal oxide coatings containing the metal precursor of the MOF. Polystyrene (PS) beads are coated with a ZnO layer to give ZnO@PS core–shell beads. The ZnO@PS beads are reactive in the presence of 2‐methylimidazole to transform part of the ZnO coating into a porous zeolitic imidazolate framework‐8 (ZIF‐8) external shell positioned above the internal ZnO precursor shell. The obtained ZIF‐8@ZnO@PS beads can be easily packed in column format for flow‐through applications, such as the solid‐phase extraction of trace priority‐listed environmental pollutants. The prepared material shows an excellent permeance to flow when packed as a column to give high enrichment factors, facile regeneration, and excellent reusability for the extraction of the pollutant bisphenol A. It also shows an outstanding performance for the simultaneous enrichment of mixtures of endocrine disrupting chemicals (bisphenol A, 4‐tert‐octylphenol and 4‐n‐nonylphenol), facilitating their analysis when present at very low levels (<1 μg L^?1) in drinking waters. For the extraction of the pollutant bisphenol A, the prepared ZIF‐8@ZnO@PS beads also show a superior extraction and preconcentration capacity to that of the PS beads used as precursors and the composite materials obtained by the direct growth of ZIF‐8 on the surface of the PS beads in the absence of metal oxide intermediate coatings.     

Synthesis and characterization of a Ni nanoparticle stabilized on Ionic liquid‐functionalized magnetic Silica nanoparticles for tandem oxidative reaction of primary alcohols

In this research, preparation of the magnetic nanoparticle, coating by a silica shell using (3‐aminopropyl) triethoxysilane and synthesis of a novel sulfonic acid‐substituted imidazolium‐based ionic liquid onto the surface of these particles via a multi‐component reaction, is described. The functionalized nanoparticles was loaded by Ni nanoparticles and characterized by means of techniques such as XRD, FTIR, SEM, EDX, TEM, TGA and ICP‐OES. The nanostructures have spherical shapes that ranged in size from 80 to 100 nm. The catalytic activity of these nanoparticles was tested in aerobic oxidation of primary alcohols that showed good performance in the wide range of primary alcohols in water at mild reaction conditions. As a second step of this work, the tandem oxidative synthesis of alkylacrylonitriles and bisindolylmethanes were investigated using primary alcohols under oxidation conditions. This catalyst system can be recovered using external magnet and reused for five consecutive cycles without significantly less of its activity.     

Efficient Oxidation of Alcohols with KBrO 3 in the Presence of Silica Chloride and Wet SiO 2

Alcohols were oxidized to their corresponding carbonyl compounds with KBrO 3 in the presence of silica chloride and wet SiO 2 , in solution and under solvent free conditions.     

Étude des Interactions du Zinc et de l'Or dans l'Étain Liquide

Abstract

Les auteurs ont étudié par voie électroehimique l'influence de faibles additions d'or sur les propriétés thermodynamiques du zinc en solution diluée dans l'étain fondu. Le paramètre d'interaction de Wagner ?_Zn ^Au et sa variation avec la température ont été déterminés dans l'intervalle de température 420–650°C: ?_Zn ^Au = 2.71 – 5.92. 10³/T.     

CaII Binding Regulates and Dominates the Reactivity of a Transition‐Metal‐Ion‐Dependent Diesterase from Mycobacterium tuberculosis

The diesterase Rv0805 from Mycobacterium tuberculosis is a dinuclear metallohydrolase that plays an important role in signal transduction by controlling the intracellular levels of cyclic nucleotides. As Rv0805 is essential for mycobacterial growth it is a promising new target for the development of chemotherapeutics to treat tuberculosis. The in vivo metal‐ion composition of Rv0805 is subject to debate. Here, we demonstrate that the active site accommodates two divalent transition metal ions with binding affinities ranging from approximately 50 nm for Mn^II to about 600 nm for Zn^II. In contrast, the enzyme GpdQ from Enterobacter aerogenes, despite having a coordination sphere identical to that of Rv0805, binds only one metal ion in the absence of substrate, thus demonstrating the significance of the outer sphere to modulate metal‐ion binding and enzymatic reactivity. Ca^II also binds tightly to Rv0805 (K_d≈40 nm ), but kinetic, calorimetric, and spectroscopic data indicate that two Ca^II ions bind at a site different from the dinuclear transition‐metal‐ion binding site. Ca^II acts as an activator of the enzymatic activity but is able to promote the hydrolysis of substrates even in the absence of transition‐metal ions, thus providing an effective strategy for the regulation of the enzymatic activity.     

Determination of water content in silica nanopowder using wavelength-dispersive X-ray fluorescence spectrometer

A wavelength-dispersive X-ray fluorescence (WDXRF) technique that uses the scattered radiation of the X-ray tube lines and the fluorescence radiation of an element present in a powder sample is proposed as a non-destructive method for the determination of the water content in silica powder. Although direct X-ray fluorescence analysis of water using WDXRF is not adequate for the quantitative determination of water in powder, due to the very low fluorescence yield for hydrogen and oxygen, the fluorescence signal of silicon (Si) in silica powder is attenuated by water, and is shown to decrease in proportion to the water content in silica powder. In addition, it is demonstrated that the Compton- and Rayleigh-scattering of the X-ray tube lines is proportional to the water content. The coefficients of determination, R², of the linear regression equations obtained from the calibration curves for all individual scattered radiations and for the fluorescence radiation of Si were > 0.90. The sum of the peak intensities of the four scattering signals, i.e. the Rayleigh-scattered Rh K–L_2,3 and Rh K–M_2,3 lines, and Compton-scattered Rh K–L_2,3 and Rh K–M_2,3 lines, also showed fairly good linearity and sensitivity over a very wide range of water content from 0 wt.% to 61.5 wt.%. However, porosity had a significant effect on the X-ray signal at low water content, in the range from 0 wt.% to 7.5 wt.%, where the sensitivity for the silica nanopowder with well-defined mesopores (~ 3 nm in diameter) decreased to 0.40 kcps/wt.%, from 0.99 kcps/wt.% for the non-porous silica nanopowder. The use of the Si fluorescence signal along with the scattered radiation of the X-ray tube lines expands the applicability of conventional XRF spectrometers to the quantitative determination of water content in silica powder.     

dl‐Aspartic Acid‐Mediated Hydrothermal Synthesis of β‐ZnS Microspheres and Their Optical Properties

ZnS hollow microspheres were synthesized by a dl ‐aspartic acid mediated hydrothermal route. dl ‐aspartic acid plays an important role as crystal growth soft template, which regulates the release of Zn²⁺ ions for the formation of ZnS hollow spheres. The formation of these hollow spheres was mainly attributed to an Ostwald ripening process. The products were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), electron diffraction (ED), UV/Vis spectroscopy (UV), and photoluminescence (PL). The shells of the microspheres were composed of ZnS quantum dots (QDs) with the average size of 2.31 nm. The average microspheres diameter is 0.5–3.5 μm. The shell thickness of the hollow sphere is ≈?300 nm. The optical bandgap energy increased significantly compared to the bulk ZnS material due to the strong quantum confinement effect. Two strong emissions at ≈?425 nm and ≈?472 nm in the photoluminescence (PL) spectrum of ZnS hollow microspheres indicate strong quantum confinement because of the presence of QDs.     

Higher‐Dimensional Unification with continuous and fuzzy coset spaces as extra dimensions

We first review the Coset Space Dimensional Reduction (CSDR) programme and present the best model constructed so far based on the , 10‐dimensional E₈ gauge theory reduced over the nearly‐Kähler manifold with the additional use of the Wilson flux mechanism. Then we present the corresponding programme in the case that the extra dimensions are considered to be fuzzy coset spaces and the best model that has been constructed in this framework too. In both cases the best model appears to be the trinification GUT .