A simple, economical and selective method employing ion pair dispersive liquid−liquid microextraction (DLLME) coupled with spectrophotometric determination of carbamazepine (CBZ) in pharmaceutical preparations and biological samples was developed. The method is based on reduction of Mo(VI) to Mo(V) using a combination of ammonium thiocyanate and ascorbic acid in acidic medium to form a red binary Mo(V) thiocyanate complex. After addition of CBZ to the complex, extraction of the formed CBZ−Mo(V)−(SCN)6 was performed using a mixture of methylene chloride and methanol. Then, the measurement of target complex was performed at the wavelength of 470 nm. The important extraction parameters affecting the efficiency of DLLME were studied and optimized in detail. At the optimum conditions, the linear range was 0.02–0.2 µg/mL. Moreover, the limits of detection and quantification were 0.01 and 0.04 µg/mL, respectively. High enrichment factor was obtained (118). Good recoveries at 0.06, 0.15 and 0.2 µg/mL ranging from 93 to 102% were achieved. The proposed method was successfully applied to the determination of CBZ in pharmaceutical formulations and biological samples.
A sensitive, accurate, and affordable colorimetric method was developed for assaying prednisolone (PRZ) in various medicinal forms. The procedure involves the oxidation of PRZ by ferric ions, followed by complexation of the resulting ferrous ions with ferricyanide to produce a greenish-blue product. Common complexation conditions were thoroughly investigated. The mole ratio of FeCl₃·6H₂O to K₃Fe(CN)₆ was 8:1. The proposed mechanism of complexation was suggested and considered. Various parameters were optimized, including the reduction of the colorimetric reaction temperature to 50°C and the duration of heating and analysis to 20-30 minutes. The calibration curve was linear over the range of 1-60 µg/mL. The limit of detection (LOD
... Show MoreThe Disi water samples were collected from different Disi aquifer wells in Jordan using a clean polyethylene container of 10-liter size. A hyper-pure germanium (HPGe) detector with high- resolution gamma-ray spectroscopy and a low background counting system was used for the identification of unknown gamma-rays emitting from radionuclides in the environmental samples. The ranges of specific activity concentrations of 226Ra and 228Ra in the Disi aquifer water were found to be from 0.302 ± 0.085 to 0.723 ± 0.207 and from 0.047 ± 0.010 to 0.525 ± 0.138 Bq L−1, with average values of 0.516 ± 0.090 and 0.287 ± 0.091 Bq L−1, respectively. The average combined radium (226Ra + 228Ra) activity and radium activity ratio (228Ra/226Ra) in Disi
... Show MoreABSTRACT : This research involves the synthesis of five to seven heterocyclic compounds starting with Schiff’s bases which derived from oxime as a starting material. 1.3-oxazepine derivatives were prepared from adding different anhydrides to the Schiff bases, tetrazole and thiazolidinone derivatives synthesized from add sodium azide and thioglycolic acid to the same Schiff’s bases as a five members ring. Pyrimidine derivatives were prepared after the reaction of the azomethine group with acetyl chloride and then urea and thiourea to synthesis on derivatives contain the six members ring. Another step included identified and confirmed these compounds by FT- IR, 1HNMR, TLC and 13CNMR finally, step included the assay of biological activity
... Show MoreThe present work includes the preparation and characterization of{Co(II) , Ni(II), Pd(II), Fe(III) , Ru(III),Rh(III), Os(III) , Ir(III) , Pt(IV) and VO(IV)}complexes of a new ligand 4-[(1-phenyl-2,3-dimethyl-3-pyrozoline-5-one)azo]-N,N-dimethylanline (PAD). The product (PAD) was isolated,studies and characterized by phsical measurements,i.e., (FT-IR), (UV) Spectroscopy and elemental analysis(C.H.N). The prepared complexes were identified and their structural geometric were suggested in solid state by using flame atomic absorption, elemental analysis(C.H.N), (FT-IR) and (UV-Vis) Spectroscopy, as well as magnetic susceptibility and conductivity measurements . The study of the nature of the complexes formed in( ethanolic solution) following t
... Show MoreA new Mannich base ligand was prepared by reacting the 2-chloro.-N-(5-mercapto-1, 3, 4-thiadazol -2-yl) acetamide and Piperidine in the presence (formaldehyde) (L) ligand. A series of ligand complexes were prepared from (L) with the metal ion Co (II), Ni (II), Cu (II), Pd (II), Pt (IV), and Au (III). Various spectroscopic techniques such as C.H.N.S, FTIR, UV-VIS, , 1HNMR, 13CNMR, Magnetic moment, and molar conductivity successfully characterize the obtained compounds. The M: L ratio was determined using the molar ratio method in solution. All prepared compounds' antibacterial and antifungal activity was studied against two types of bacteria and one type of fungi at a rate of 0.02M. The standard ΔH° f and ΔEb of the ligands an
... Show MoreTwo quantitative, environment-friendly and easily monitored assays for Ni (II) and Co (III) ions analysis in different lipstick samples collected from 500-Iraqi dinars stores located in Baghdad were introduced. The study was based on the reaction of nickel (II) ions with dimethylglyoxime (DMG) reagent and the reaction of cobalt (III) ions with 1-nitroso-2-naphthol (NN) reagent to produce colored products. The color change was measured by spectrophotometric method at 565 nm and 430 nm for Ni and Co, respectively, with linear calibration graphs in the concentration range 0.25-100 mg L-1 (Ni) and 0.5-100 mg L-1 (Co) and LOD and LOQ of 0.11 mg L-1 and 0.36 mg L-1 (Ni), and 0.15 mg L-1 an
... Show MoreA new simultaneous spectrophotometric-kinetic method was developed to determine phenylephrine (PHEN) and tetracycline (TETR) via H-point standard addition method (HPSAM). The proposed procedures rely on the measurements of the difference in the rate of charge-transfer (CT) reaction between each of PHEN and TETR as electron donors with p-Bromanil (p-Br) as an electron acceptor. Different experimental factors which affect the extent of the complex formation were investigated by monitoring the value of absorbance at 446 nm. Time pair of 50 -100 sec was selected and employed, among different examined pairs since it results in the highest accuracy for HPSAM-plot. Linear calibration graphs in the concentration ranges of 10.0-40.0 and 10.0–50.0
... Show MoreA novel azo dye ligand namely (2-(pyridin-3-yldiazenyl)naphthalen-1-ol (HPYNA), was synthesized by the coupling reaction of diazonium salt of 3-aminopyridine with naphthol. The palladium(II) complex for HPYNA ligand was prepared by reacting palladium(II) ions with the HPYNA ligand. These synthesized compounds were characterized using different techniques, including mass, 1H-NMR, infrared, and UV-Vis spectroscopy. The infrared results show that the azo ligand reacts as a bidentate via the oxygen atom of phenol and nitrogen atom of the azo group. The palladium(II) complex is square-planer with diamagnetic properties depending on the results of electronic transitions and magnetic sensitivity. The HPYNA ligand and palladium complex show
... Show MoreChukar partridge Alectoris chukar (Gray, 1830) is the only species of the 46 species of the genus Alectoris to be found in Iraq. At least there are fourteen subspecies of chukar were described from east Europe, the Middle East and west Asia, two of them were known to be found in Iraq, A.c. Kurdestanica (Meinertzhagen, 1923) from Alpine bio-geographical zone of altitude more than 2000m high, and A.c. werae Zarundny and Loudon, 1904, from the foothills of altitude not more than 400m. In between these two regions, there is another bio-geographical region known as the Irano-toranian zone 400-2000m high. Using morphological, ecological, behavioural, reproduction and hybridization criteria this study discove
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