A simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions, the linearity ranges of calibration curves were 1-9 and 0.5-8 µg/mL with detection limits of 0.26 and 0.09 µg/mL of ISX for batch and CPE methods respectively. A relative standard deviation (RSD %) best than 1.98 and 2.67 % with the percentage recoveries range 100.14 and 99.63 % were obtained for both methods respectively. The proposed methods were successfully used in routine analysis of ISX in pharmaceutical forms with high accuracy and reproducibility.
In the present study, a novel ligand (L) made of 2-hydroxynaphthaldehyde and 3-hydrazone-1,3-dihydro-indole-2-one(3-[(3-hydroxynaphthalen-2-yl-ethylidene)-hydrazono]-1,3-dihydro-indol-2-one). The ligand was characterized by FTIR, UV-vis, mass, 1H-NMR, 13C-NMR, and CHN elemental analysis. New complexes of this ligand were created by treating methanol and a drop of DMF solution of the produced ligand with the hydrated metal salts of Mn(II), Co(II), Ni(II), Cu(II), and Zn(II) in a molar ratio of 2:1 (L:M). As a result, complexes have been emerged and identified FTIR, UV-vis, C.H.N., chloride-containing, molar conductance, magnetic susceptibility, and atomic absorption. The characterization result for each complex indicated complexes wi
... Show MoreThe new azo dye was synthesized via the reaction of the diazonium salt form of 3-aminophenol with 2-hydroxyquinoline. This dye was then used to access a series of complexes with the chlorides of manganese, iron, zinc, cadmium, and vanadium sulfate. The prepared ligand and its complexes were characterized by FT-IR spectroscopy, UV-visible spectroscopy, mass spectrometry, thermogravimetric analysis, differential scanning calorimeter, and microelemental analysis. Conductivity, magnetic susceptibility, metal content, and chlorine content of the complexes were also measured. The ligand and cadmium complex were identified using1H NMR and 13C NMR spectroscopy. The results showed that the shape of the ligand is a trigonal planner, and the c
... Show MoreAddition chloro acetyl isothiocyanate (C3H2ClNOS) with 3-Aminoaceto phenone (C8H9NO) to prepare a fresh Ligand [N-(3-acetyl phenyl carbamothioyl)-2-chloroacetamide](L). The ligand (L) behaves as bidentate coordinating through O and S donor with metal ions, the general formula of all complexes [M(L)2(Cl)2](M+2 = Manganese(II), Cobalt(II), Cadmium(II) and Mercury(II)). Compounds were investigation by Proton-1, Carbon -13 NMR spectra (ligand (L) only), Element Microanalysis for C, N, H, O, S, Fourier-transform infrared, UV visible, Conductance
This work involves synthesis of some new heterocyclic compounds including 1, 3-diazetine. The new Schiff bases [VI] ad derived from 3-((5-hydrazinyl-4-phenyl-4H-1, 2, 4-triazol-3-yl) methyl)-1H-indole [V] which was synthesized by refluxing 5-((1H-indol-3-yl) methyl)-4-phenyl-4H-1, 2, 4-triazole-3-thiol [IV] with hydrazine hydrate in absolute ethanol and this amino compound [V] condensation with different aromatic aldehydes in absolute ethanol to yielded a new Schiff bases [VI] ad. N-acyl compounds [VII] ad were synthesized by addition reaction of acetyl chloride to imine group of Schiff bases in dry benzene. The new diazetine derivatives [VIII] ad synthesized by the reaction of N-acyl compounds [VII] ad with sodium azide in dimethylformamid
... Show MoreThis work represents the preparation of the starting material, 3-chloro-2-oxo-1,4-dithiacyclohexane (S) using a new method. This material was reacted with, 4-phenylthiosemicarbazide to give (H3NS3) as a tetradentate ligand H3L. New complex of rhenium (V) with this ligand of the formula [ReO(L)] was prepared. New complexes of the general formula [M(HL)] of this ligand when reacted with some metal ions where: M = Ni(II), Cu(II), Cd(II), Zn(II), Hg(II) have been reported. The ligand and the complexes were characterized by infrared, ultraviolet–visible, mass, 1H nuclear magnetic resonance and atomic absorption spectroscopic techniques and by (HPLC), elemental analysis, and electrical conductivity. The proposed structure for H3L with Re (V) i
... Show MoreThe compound [L] was produced in the current study through the reaction of 4-aminoacetophenon with 4-methoxyaniline in the cold, concentrated HCl with 10% NaNO2. Curcumin, several transition metal complexes (Ni (II), La (III), and Hg (II)), and compound [L] were combined in EtOH to create new complexes. UV-vis spectroscopy, FTIR, AA, TGA-DSC, conductivity, chloride content, and elemental analysis (CHNS) were used to describe the structure of produced complexes. Biological activities against fungi, S. aureus (G+), Pseudomonas (G-), E. coli (G-), and Proteus (G-) were demonstrated using complexes. Depending on the outcomes of the aforementioned methods, octahedral formulas were given as the geometrical structures for each created comp
... Show MoreThe reaction of 2-amino benzoic acid with 1,2-dichloroethane under reflux in methanol and KOH as a base to gave the precursor [H4L]. The precursor under reflux and drops of CH3COOH which reacted with (2mole) from salicycaldehyde in methanol to gave a new type N2O4 ligand [H2L], this ligand was reacted with (MCl2) Where [M= Co (II), Ni(II), Cu(II) and Zn(II)] in (1:1) ratio at reflux in methanol using KOH as a base, to give complexes of the general formula [M(L)]. All compounds have been characterized by spectroscopic methods [1H NMR ( just to the ligand), FTIR, uv-vis, atomic absorption], melting point, conductivity, chloride content, as well as magnetic susceptibility measurements. From the above data, the proposed molecular structu
... Show MoreThe complexes of the 2-hydroxy-4-Nitro phenyl piperonalidene with metal ions Cr(III), Ni(II), Pt(IV) and Zn(II) were prepared in ethanolic solution. These complexes were characterized by spectroscopic methods, conductivity, metal analyses and magnetic moment measurements. The nature of the complexes formed in ethanolic solution was study following the molar ratio method. From the spectral studies, monomer structures proposed for the nickel (II) and Zinc (II) complexes while dimeric structures for the chromium (III) and platinum (IV) were proposed. Octahedral geometry was suggested for all prepared complexes except zinc (II) has tetrahedral geometry, Structural geometries of these compounds were also suggested in gas phase by using
... Show MoreLimitations of the conventional diagnostic techniques urged researchers to seek novel methods to predict, diagnose, and monitor periodontal disease. Use of the biomarkers available in oral fluids could be a revolutionary surrogate for the manual probing/diagnostic radiograph. Several salivary biomarkers have the potential to accurately discriminate periodontal health and disease. This study aimed to determine the diagnostic sensitivity and specificity of salivary interleukin (IL)‐17, receptor activator of nuclear factor‐κB ligand (RANKL), osteoprotegerin (OPG), RANKL/OPG for differentiating (1) periodontal health from disease and (2) stable a