Diazotization reaction between 1-(2,4,6-trihydroxy-phenyl)-ethanone and diazonium salts produced the ligand 4-(3-Acetyl-2,4,6-trihydroxy-phenylazo)-N-(5-methyl-isoxazol-3-yl)- benzenesulfonamide, which in turn reacted with the metal ions (Ni2+, Zn2+, Pd2+ and Pt4+) forming stable complexes with Octahedral geometry suggest of (Ni2+ and Pt4+), Zn2+ complex Tetrahedral and Pd2+ complex Square planer. The creation of such complexes was detected by employing spectroscopic means involving ultraviolet-visible, which proved the obtained geometries; FT-IR confirmed the formation of the azo group and the coordination with metal ions through it. Thermogravimetric analysis studies demonstrated the coordination of water residues (aqua or hydrate) with metal ions inside the coordination sphere, as well as used curve DSC to calculate the thermodynamic parameters ΔH, ΔS, and ΔG. Moreover, element microanalysis and atomic absorption gave corresponding outcomes with theoretically counting outcomes. Neuclearmagnatic resonances for 1H and 13C, chlorine atoms, and magnetic moment quantifications also indicate the formation of azo dye ligand. The ligand and new complexes showed antioxidant abilities to scavenge free radicals
This paper describes the development of a simple spectrophotometric determination of bismuth III with 4-(2-pyridylazo) resorcinol (PAR) in aqueous solution in the presence of cetypyridinium chloride surfactant at pH 5 which exhibits maximum absorption at 532 nm. Beer's law is obeyed over the range 5-200 µg/25 mL. i.e. 0.2-8 ppm with a molar absorptivity of 3×104 l.mol-1.cm-1 and Sandell's sensitivity index of 0.0069 µg.cm-2. The method has been applied successfully in the determination of Bi (III) in waters and veterinary preparation.
The Reversed Phase High Performance Liquid Chromatography (RP-HPLC) has been used for the separation of Poly aromatic hydrocarbons(PAHs) by using column Reprosil 100 C 18 which was found to be a suitable one for this purpose. The result showed that using mobile phase of (Acetonitrile-water) Reversed Phase HPLC , flow rate of (1.2 ml/min) , column temperature (30CËš) and wave length of (254nm), give a complete separation with a good resolution . The total separation time was less than 20 min. The result of the study showed that the vegetables of Baghdad city were polluted by poly aromatic hydrocarbons(PAHs) in different places where samples taken because of drainage of the heavy water ,industrial trash and trash of oil colanders. -
... Show Moreprotein oxidation through oxidative stress, which represents the overall status of the protein in the cell/tissue. Due to their increased levels of AOPPs were reported during T2DM. The aim of this study was to assess AOPP level in T2DM subjects with foot ulcer (DFU) and explore its correlation with infection. Type 2 diabetic patients (n=108) and healthy subjects (n=25) were enrolled in this study. The T2DM group was subdivided to diabetic patients without complications (n=25) and eighty-three (83) of them have diabetic foot. They were sub- grouped into two groups according to presence Osteomyelitis and abscess, and in reliance on medical analysis of WBC count and CRP. Group of diabetic without superficial or deep ulcer and no osteomyelitis
... Show MoreA spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and l
... Show MoreA rapid high performance liquid chromatography method for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by employing a silica-based monolithic column is described. The samples were first extracted using ethyl acetate and derivatized using ortho-phthaldialdehyde in the presence of 2-mercaptoethanol. C20 sphinganine was used as internal standard. Under the optimized conditions, separation was achieved using a mixture of methanol:water (93:7, v/v), column temperature at 30°C, flow rate of 1 mL min−1, and an injection volume of 10 μL. Good linearity was obtained for Sa and So over the concentration range 20–500 ng mL−1(correlation coefficients ≥0.9978). The detection limits were 0.45 ng mL−1 for Sa and
... Show MoreA solid Phase Extraction (SPE) followed by HPLC-UV method is described for the simultaneous quantitative determination of nine priority pollutant phenols : Phenol, 2- and 4-Nitrophenol, 2,4-Dimethylphenol, 2-, 2,4-Di-, 2,4,6-Tri-, and Penta- chlorophenol, 4 Chloro-3-methylphenol. The phenols were separated using a C-18 column with UV detector at wave length of 280nm. The Flow of mobile phase was isocratic consisted of 50:50 Acetonitrile: phosphate buffer pH=7.1, column temperature 45 C°, Flow Rate 0.7 ml/min. Calibration curves were linear (R2 = 0.9961-0.9995). The RSDs (1.301-5.805)%, LOD(39.1- 412.4) µg/L, LOQ(118.5-1250.8) µg/L, the Robustness (1.55-4.89), Ruggedness (2.82-4.00), Repeatability (2.1-4.95), Recoveries%
... Show MoreSimple, precise and economic batch and flow injection analysis (FIA)-spectrophotometric methods have been established for simultaneous determination of salbutamol sulfate (SLB) in bulk powder and pharmaceutical forms. Both methods based on diazotization coupling reaction of SLB with another drug compound (sulfadimidine) as a safe and green diazotization agent in alkaline medium. At 444 nm, the maximum absorption of the orange azo-dye product was observed. A thorough investigation of all chemical and physical factors was conducted for batch and FIA procedures to achieve high sensitivity. Under the optimized experimental variables, SLB obeys Beer’s law in the concentration range of 0.25-4 and 10-100 μg/mL with limits of detection o
... Show MoreIn this study, simple, low cost, precise and speed spectrophotometric methods development for evaluation of sulfacetamide sodium are described. The primary approach contains conversion of sulfacetamide sodium to diazonium salt followed by a reaction with p-cresol as a reagent in the alkaline media. The colored product has an orange colour with absorbance at λmax 450 nm. At the concentration range of (5.0-100 µg.mL-1), the Beer̆ s Low is obeyed with correlation coefficient (R2= 0.9996), limit of detection as 0.2142 µg.mL-1, limit of quantification as 0.707 µg.mL-1 and molar absorptivity as 1488.249 L.mol-1.cm-1. The other approach, cloud point extraction w
... Show MoreThe current study aimed to evaluate the effect of the heavy metals copper, cadmium and cobalt when added individually, in combination and in combination on the growth and reproduction of the aquatic fungus Saprolegnia hypogyna.
The leaves and stems of the local Purslane plant ( Portulaca oleracea oleracea L. ) were used to preapare the extract of two types ( wet and dried extractions) the extracts were prepared by weighting of 60grams of the wet and the dried plant individually, then boiled in 500ml of distal water. Finally the volume was completed to1 liter, then we used these extracts to prepare of 8 types of the culture media contained basic, selective and enrichment media for growing a group of pathogenic bacteria. 8 types of bacteria were used for this purpose: Escherichia coli, Pseudomonas flouresence, Staphylococcus aureus , Staphylococcus epidermidis, Bacillus subtilis , Klebsiella pneumoniae , Proteus mirabilis and Proteus vulgaris. The stastica
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