Rafidain Journal of Science

The study has focused on obesityin women with Polycystic Ovary Syndrome (PCOS), as a potential new indicator of infertility by evaluating twelve biochemical and hormonal variables such asprogesterone, estrogen, Follicle Stimulating Hormone (FSH), LH/FSH ratio, Luteinizing hormone (LH), Thyroid Stimulating Hormone (TSH), Prolactin, Cholesterol, Triglyceride (TG), Very Low Density Lipoprotein (VLDL). High Density Lipoprotein (HDL) and Low Density Lipoprotein (LDL). In all women, biochemical and hormonal tests have been examined. The effect of Waist to Hip ratio (WHR) and Body Mass Index (BMI) has been evaluated. The correlation between being afflicted with PCOS and WHR has been found to be positively correlated with LH, LH/FSH ratio, TSH, Cholesterol, TG, LDL and VLDL, whereas the negative correlation with estrogen, progesterone, FSH and HDL. Therefore, we conclude that WHR and BMI are new Indexes in obesity, indicating the increase of infertility with PCOS risk..

Unsymmetrical Schiff baseH2L1=2-((8-((E)-1-((2-hydroxy phenyl) ethylidene amino) naphthalen-1-ylimino) methyl)-6-methoxyphenol and H2L2=1-((E)-(8-((E)-1-(2-hydroxy phenol) ethylidene amino) naphthalen-1-ylimino)methyl)naphthalen-2-ol which derived from 1,8-diaminonaphthalene and 2-hydroxy acetophenone and then with 2-hydroxy-3-methoxy benzaldehyde or 2-hydroxy-1-naphthaldehyde and their complexes of the type [M Ln], where n=1,2 and M=Co(II) Ni(II),Cu(II)and Zn(II) have been synthesized. Adduct complexes of the type [MLn(py)2] were also prepared in(1:2)(complex: py) molar ratio. The complexes and adducts were characterized by elemental analysis (C.H.N), metal content, (IR,UV-Vis,1H-NMR)spectroscopy, conductivity and magnetic measurements. The resulting data suggested that the Schiff bases containing ONNO donor atoms act as dibasic tetradentate ligands through coordination with metal ions. Conductivity data in DMF solution showed that all complexes are non-electrolyte. Magnetic moment and electronic spectra dada indicate that the complexes have either squar planer or octahedral geometry, the ligands and their complexes gram negative bacteria (Salmonella typhi andEscherichia coli)

Unsymmetrical Schiff bases H2L1 = [ 1- (( E )-(( 3-((( E) -2- hydroxybenzylidene) amino)phenyl)imino)methyl) naphthalene-2-ol] and H2L2 = [1-((E)-((3-(((E)-1-(2-hydroxphenyl)
ethylidene ) amino ) phenyl ) imino ) methyl ) naphthalene - 2 – ol ] which derived from m - phenylenediamine and 2-hydroxynaphthaldehyde and then with salicyaldehyde or 2- hydroxyacetophenone, and their complexes of the type [M 2Ln 2], where n = 1, 2 and M = Mn(II), Co(II), Ni(II) and Cu(II) have been synthesized. Adduct complexes of the type [M2Ln 2 (py)4] were also prepared in (1 : 4)(complex : py) molar ratio. The complexes and adducts were characterized by elemntal analysis (C. H. N), metal content, (IR, UV- v.s, 1H-NMR) spectroscopy, conductivity and magnetic measurements. The resulted data suggested that the Schiff bases containing ONNO donor atoms acts as dibasic tetradendetate ligands through coordinated with metal ions. Conductivity data in DMSO solution showed that all complexes are non- electrolyte. Magnetic moment and electronic spectra data indicat that the complexes have either tetrahedral or octahedral geometry while [Ni2 Ln 2] complexes have square planer geometry. The legends and their complexes were screened for antibacterial activity against Staphylococcus- aureus and Escherichia coli. The ligands and their complexes showed some biological activities
.

A series of heterocyclic compounds containing oxygen and nitrogen atoms, isoxazoline ІI(a-d) and another containing two nitrogen atoms, pyrazolinesІII(a-d) and phenylpyrazolines IV(a-d) were prepared by the reaction of a proper azachalcones І(a-d) with hydroxylaminehydrochloride, hydrazine hydrate or phenylhydrazine. These heterocyclic compounds were characterized by 1H-NMR , CHN , IR and UV spectra in addition to their some physical properties. Also, these prepared compounds were screened for their biological activities and a theoretical calculation which shows that the product IVa obtained from 1,2 – rout was energetically more stable by 1.3967 kcal/mole than that came from 1,4 – rout, thus the reaction proceed via 1,2 – addition 1,2)).

A simple and sensitive spectrophotometric method is proposed for the determination of mesalazine (MZ) in some of its pharmaceutical preparations. The method is based on the diazotization of mesalazine by reaction with sodium nitrite in an acidic medium and then coupling of diazonium salt corresponding to mesalazine with 2,6-dihydroxytoluene reagent in basic medium to produce an intense orange colored water-soluble and stable azo-dye for at lest two hrs, and exhibits maximum absorption at 453 nm. Beer’s law is obeyed in the concentration range of 2.5-100 µg of mesalazine in a final volume of 10 ml i.e.,0.25-10.0 ppm with a molar absorptivity of 4.6×104 l. mol-1. cm-1 and sandell sensitivity index of 0.00332 µg. cm-2 . A relative error is -0.48 to -4.80 and relative standard deviation of ±0.01 to ±0.17 depending on the concentration level. The proposed method has been applied successfully to determine mesalazine in pharmaceutical preparations, tablets and suppositories.

.

An indirect spectrophotometric method for the determination of chloramphenicol (CAP) has been suggested. The method is based on the oxidative coupling reaction of reduced chloramphenicol (R-CAP) with 2,7- dihydroxynaphthalene (2,7-DHN) reagent in the presence of potassium dichromate as oxidizing agent to produce brown colored, stable and soluble product. This product showed maximum absorption at 544 nm. Beer’s law is obeyed over the range 0.5-7.5.µg.ml-1 of R – CAP and molar absorptivity of 1.069×105 l.mol-1.cm-1 and Sandell's sensitivity index of 0.0030 µg.cm-2, limit of detection (LOD), limit of quantitation (LOQ), relative error (RE%) and relative standard deviation (RSD%) have been estimated. The method has been successfully applied to the determination of CAP in drug formulations

In this work an electrochemical behavior quantification and interaction of valsartan and glibenclamide were studied using square wave voltammetric technique. The effect of temperature on the interaction was investigated and the thermodynamic parameters (∆H, ∆S & ∆G) were calculated for the interaction and binding constant (K) also obtained. The calibration curves of each drug were linear within the range of concentration [(4.99×10-7) – (6.95×10-6)], [(5.96×10-8) – (1.15×10-6)] molar with R2 value equal to 0.9819, 0.9926 for valsartan and glibenclamide respectively..

An accurate, simple, and sensitive indirect spectrophotometric method which proposed and developed for the determination of paracetamol in different pharmaceutical preparations. The proposed method was based on acid hydrolysis of PAR to produced p-aminophenol (PAP), PAP was diazotization with nitrite ion to form the corresponding diazonium salt, followed by coupling with histidine reagent in alkaline medium to produced azo dye that showed maximum absorbance at 430 nm. Beer's law was obeyed in the concentration rage of 10-500 µg/20 ml (i.e. 0.5-25 ppm). The molar absorpitivity and Sandell's sensitivity of the dye were. 1.118×104 l.mol-1.cm-1and 0.0135 µg.cm-2 respectively. The method successfully has been applied for the determination of PAR in pure form,and its pharmaceutical preparations (tablets, syrup and injection).

).

An indirect method for the estimation of fluoride ion has been developed.The method is based on the bleaching action of fluoride ion on the color of Ti (IV)with 2-hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo)-3-naphthanic acid (HHSNNA) complex with proportional decrease of absorbance. Therefore,the decrease in color intensity is proportionalto the concentration of fluoride ion. Molar absorptivityis 0.1166×104 l. mol-1.cm-1 atwavelength 685 nm. Beer's lawis obeyed over the concentration range of 0.2-4 µg/ml.The proposed method is applied successfullyto determine fluoride ion in different real water samples andpharmaceutical preparations (Tablets). The proposed method is compared favorably with Eriochrome cyanine R – Zirconium method .

One side of (o, m and p) benzene diamine reacted with aromatic aldehyde to give Schiff bases (Ia-d) or (IIa-d) and (IIIa-d) respectively. The second amine group of the synthesized Schiff bases (Ia-d or IIa-d and IIIa-d) was reacted with substituted-9-chloroacridine to give the final compounds namely N-(Substituted benzylidene )-N'-(Substituted acridine -9-yl) (1,2 or 1,3 and 1,4) benzene diamine (V,VI,VII).The reaction progress was followed by thin layer chromatography (TLC), and Rf values were recorded. I.R. Spectral data for all the synthesized derivatives were reported. The U.V-Vis., and the 1HNMR(300and 400MHz) were recorded for some derivatives to support the structure of the synthesized compounds. .

A new series of complexes of Co(II), Ni(II), Cu(II), and Zn(II) with three hydrazones ligands(L) derived from 2-hydroxy-4-methoxy acetophenone (Paeonol) and 4-methylbenzoylhydrazide (AMBH), acetyl hydrazine (AAH), or picolinoyl hydrazine (APH) with the general formula [M(L-H)2].nH2O (n= 0, 1, or 2) where L-H = deprotonated AMBH, AAH or APH, have been prepared and characterized by elemental analyses, spectral (FT-IR, UV–visible) as well as molar conductance and magnetic measurements. The data revealed that the ligands AMBH and AAH act as mono-negative ONO chelates coordinated through the carbonyl group and the phenoxy oxygen atoms and azomethine nitrogen atom, while APH acts as NNO chelate, coordinated through the pyridine and azomethine nitrogen atoms and the phenoxy oxygen atom. On the basis of electronic spectral and magnetic moment data, an octahedral geometry is suggested for all complexes. Also, the ligands and some of their complexes were screened for antibacterial activities.

A number of new Co(II), Ni(II), Cu(II) and Zn(II) complexes with 2,5-hexanedione bis(4-methylbenzoyl hydrazone)(HDMBH), 2,5-hexanedione bis(2-theonyl hydrazone)(HDTH) and 2,5-hexanedione bis(2-furoyl hydrazone)(HDFH) have been reported.The bis-hydrazone ligands were synthesized by the condensation of 2,5-hexanedione with (4-methylbenzoic acid hydrazide,2-thiophene carbohydrazide or 2-furic acid carbohydrazide) in 1:2 molar ratio. The reaction of metal(II) chlorides with the ligands in (1:1) molar ratio in ethanol in presence of triethylamine lead to the isolation of complexes having the general formula [M(L-2H)(H2O)2] where (M= Co(II), Ni(II), Cu(II) and Zn(II)) and (L-2H=doubly deprotonated ligand). The ligands and complexes have been characterized by elemental analysis, spectral (IR,UV-Vis), magnatic and molar conductance measurements, which revealed that the ligands HDMBH, HDTH, and HDFH act as dinegtive charge tetradentate (NNOO-2) donor ligands in the metal complexes, coordinated through the two azomethine group nitrogen atoms and the two enolic oxygen atoms. All complexes provide an octaheadral geomatry..

In this work, the interaction between theophylline (TP) which gives a stable well-defined reduction peak at (1.07) V versus Ag/AgCl. Sat. KCl/ in phosphate buffer solution (pH=7) and urea was studied using square wave voltammetry (SWV) technique. Also, the binding constant and the thermodynamics parameters have been calculated. Different temperatures (288, 293, 298, 298, 303, 308 and 310) ºK were used to study the effect of temperature on binding constant (K). The results showed that the binding constant (K) decreased with increasing temperature. This is as a result of the negative value of enthalpy (-31.07)KJ.mol-1. The negative value of Gibbs energy (-13.632 x 102_ -12.296 x 102) KJ.mol-1 indicates that the interaction is spontaneous and could be due to van der Waals forces or hydrogen bonds effect (weak interaction).).

Mesalazine (MESA) is determined by a simple and rapid visible spectrophotometric method. This method is depend on oxidative coupling reaction of mesalazine with histidine (HIS) in alkaline media using N-bromosuccinimide (NBS) as oxidizing agent to form a water soluble and stable product, that it has a maximum absorption at 459 nm. Beer's law is followed in a concentration range of 50 to 750 μg /20ml (2.5-37.5 μg /ml) with a molar absorptivity of 3.3682×103 l.mol-1. cm-1. The recommended method has been successfully applied to the assay of MESA in pharmaceutical preparations.

The 2-[(6-chloro-2-pyridyl) amino]benzoic acid (I) was synthesized viaUllmann-Goldberg coupling by reaction of anthranilic acid with2,6-dichloropyridine. The compound (I) was cyclized by using poly phosphoric acid (PPA) to give 9-chloro-11H-pyrido[2,1-b]quinazolin-11-one (II). The compound (II) reacted with hydrazine hydrate to give N-{11H-pyrido[2,1-b]quinazolin-11-one-9-yl} hydrazine (III). The compound (III) reacted with various aromatic aldehydes to yield the hydrazones (IVa-p). The reaction progress was followed by thin layer of chromatography (TLC). The physical constants and Rf values were recorded. The synthesized compounds were confirmed via the spectral data (UV,I.R,1H-NMR, 13C-NMR, mass spectra). The possible fragmentation pattrene of GC/MS for the compounds (IVa) were investigated (IVh).).

A simple, rapid, accurate and sensitive spectrophotometric method for the determination of thiamine has been developed. The method is based on the direct reaction between thiamine and sodium hydroxide to produce a yellow colored product having maximum absorption at 335 nm. Beer's law was obeyed over the concentration range of 2-20µg/ml,with molar absorptivity of 1.58x104 l/mol.cm. The present method was considered to be simple because it does not need heating, hydrolysis and solvent extraction steps. The ingredients often formulated with thiamine, have been shown not to interfere, and is suitable for the routine determination of thiamine. The proposed method has been successfully applied for the determination of thiamine in pure form and in pharmaceutical preparations(tablets).

).

Electrochemical biosensor is an effective tool for pharmaceutical analysis due to its simplicity, specificity, sensitivity, fast, cost effective and repetitive measurements with miniaturized and portable devices. The paper illustrates the detail methodology for development of an electrochemical biosensor based on hemoglobin (Hb) film modified for anticancer drug adriamycin (ADM). Square wave voltammetry (SWV) studies of the electrodes before and after immobilizing of HB shows the successful formation of a selectivity of the electrode. The proposed Hb based biosensor allows quantitation over the range 1 to 8010-8M, The suggested biosensor method can be successfully applied to the detection and determination of anticancer drug adriamycin in different drug formulations and can be suggested as a suitable sensor for analysis of Adriamycin in biological samples.ً.

The purpose of this study was to characterize the physical behaviour of Dura asphalt modified by styrene-butadiene-styrene (SBS)co-polymer. The polymer modified asphalt (PMA) was produced by mixing a 40/60 penetration grade Dura (base) asphalt withdifferent ratios of the copolymers. The resultsthus exhibited that the modification of the authentic asphalt by SBS had great impact on the physical properties of the asphalt. Furthermore, the high temperature performance of the original asphalt was enhancedsuch that the morphology observed by microscope examinationrevealed the compatibility between SBS and asphalt. Additionally,the storage stability of the binder was significantly improved in comparison with Dura asphalt..

The voltammetric behavior of Thyroxine (T4) was studied using square wave voltammetry in phosphate buffer solution at (pH 7.0) as supporting electrolyte. Thyroxine gives two well-defined reduction peaks at Ep1 (-0.359) volt and Ep2 (-1.01) volt versus the reference electrode (Ag/AgCl/Sat.KCl). The calibration curve is linear within a two range of concentration, first is (1.996x10-7 - 19.61x10-7)M with the R2 equal to (0.999) and (0.9963) for Ep1 and Ep2 respectively, and second (0.996x10-6 - 11.857x10-6) M with the R2 equal to (0.9819) and (0.9848) for Ep1 and Ep2 respectively. The Gibb`s free energy (ΔG), enthalpy (ΔH) and entropy (ΔS) changes of temperature dependent on (K) were calculated using Van`t Hoff equation for Thyroxine and Thiourea binding. The molecular docking between Thyroxine and Thioureahas been studied, and the results indicates thatthe interaction between T4 and TU was mainly hydrogen bonding and van der Waal`s interaction..

The voltammetric behavior of Thyroxine (T4) was studied using square wave voltammetry in phosphate buffer solution at (pH 7.0) as supporting electrolyte. Thyroxine gives two well-defined reduction peaks at Ep1 (-0.359) volt and Ep2 (-1.01) volt verses (Ag/AgCl/Sat.KCl) as reference electrode. The Gibb`s free energy (ΔG), enthalpy (ΔH) and entropy (ΔS) changes of temperature dependent on (K) were calculated using Van`t Hoff equation for Thyroxine and Uracil binding. The molecular docking between Thyroxine and Uracil has been studied, and the results indicate that the interaction between T4 and Ur was mainly hydrogen bonding and van der Waals interaction.

The interactions of Co-enzyme Q0 with Aniline and Pyrrole were studied in aqueous phosphate buffer solution at (pH=7.0) as supporting electrolyte using square wave voltammetry, Co-enzyme Q0 gives a well-defined square wave voltammetric peak at (-0.0415) volt against the reference electrode (Ag/AgCl/3M KCl). The binding constants (K) were calculated at different temperatures. Vant's hoff equation is applied to calculate the thermodynamic parametrs (ΔH enthalpy changes, ΔS entropy changes and ΔG free energy changes), and then the type of interaction was estimated. The results indicated that the interaction between Co-enzyme –Q0 and Aniline (ΔH and ΔS negative values) was probably due to Vander Waals forces or hydrogen bonding interaction, and the second interaction between Co-enzyme-Q0 with Pyrrole (ΔH and ΔS positive values) might be due to the hydrophobic interaction .

The work reported deals with the preparation and characterization of a number of new complexes of manganese (II). The complexes are formed by the reaction of the mentioned metal salts with three ligands of Schiff base type; the ligands are: dibenzoinlidenemalonoyldihydrazide (L1‌H4), dibenzoinlidenesuccinyldihydrazide (L2H4) and dibenzoinlidenephthalolyldihydrazide (L3H4). The prepared complexes have been characterized by molar conductance, CHN analysis, metal contents,electronic spectra, infrared spectra, and magnetic susceptibility measurements.The different studies suggest that all the complexes are hexacoordinated with octahedral geometry in the neutral medium; the ligands formed cationic complexes of the type [Mn(LH4)]X2 were X=Cl-1and NO3-1 , while in a basic medium anionic complexes of the general formula K2[Mn(L)]. K2[Mn(L)].

Carboxy methyl cellulose, pectin, chitosan or acrylic acid– poly (vinyl alcohol) blend hydrogels were prepared using Glutaraldehyde (GLU) as chemical or sodium hexameta phosphate (SHMP) as physical cross-linking agent. The prepared hydrogels have carried the advantage properties of both blend materials and can be used for loading and releasing of BSA protein. The degree of swelling of the prepared hydrogels was measured due to their different functional groups in different pHs of (pH4, pH7 and pH9) in addition to the electrolyte solution of 0.1 N NaCl. The blend hydrogels are characterized for their chemical structure using FT-IR. The XRD analysis was investigated for determination of the hydrogels crystallographic structure. The differential thermal analysis DTA and scanning electron microscope SEM were depended to study the thermal stability and surface morphology of the hydrogel respectively. The hydrogels were loaded with BSA protein model, and time of loading at (1.5, 3.0, 4.5 and 6.0) hrs were measured, beside the pH of the loading solution of ph4, pH6 and pH8 were considered and the BSA concentrations of (0.5, 1.0, 1.5 and 2.0) g/L have been investigated for maximum loading percentages %Lmax of BSA on the hydrogels. Finally the loaded BSA was released under different release conditions in 0.9% w/vNaCl solution and pH4, pH6 and pH8 were depended and the BSA was tested to release at 15, 25 and 40oC releasing medium temperatures. (15, 25 and 40)oC.

Xanthatecomplexes of the general formula [M{Ag(oleylXant)2}2] (A) and [MM'(oleylXant)4] (B) were M = Copper (II), Nickel II), Cobalt (II) M' = Cadmium(II), Zinc(II). These complexes were reacted with bidentatelewis base (1,10-phenanthroline). The result of this reaction gave the complexes [M(phen)][{Ag(oleylxant)2}2] (I.A) and [M(phen)][M'(oleyl-xant)4] (I.B), which have been prepared and measured by an infrared, magnetic suscetptibility measurements, conductance measurements, electronic spectra and elemental analysis electronic absorption spectra. These data indicate gave the result that the complexes of the type (A & B) are a square planer geometry while the complexes of the type (I.A), (I.B) have an octahedral geometry.

.

The research involved clinical study of rhodanese enzyme and its relation with some biochemical parameters in renal failure.
The result demonstrated a significant increase in the activity of rhodanese and metallo-endopeptidase and in concentration of urea, and potassium while a significant decrease activity of sulfate oxidase, thiosulfate oxidase and arylesterase and in concentration of albumin and sodium in renal failure patients compared with control.
The results also demonstrated a significant decrease in the activity of rhodanese in male compared with female in each of patients and control groups.
Correlation coefficients between rhodanese and biochemical parameters of renal failure patients showed that activity of rhodanese has negative correlation with activity of sulfate oxidase, thiosulfate oxidase and concentration of albumin while appositive correlation with activity of metallo –endopeptidase and concentration of urea in renal failure patients.
These results provide evidence of a major role for rhodanese enzyme in renal failure, which led to consider it as a marker for renal failure and its relation with biochemical parameters in patients group.
.

The study was accomplished for the evaluation of the efficiency of the processing station of excretion in Al – Qayyarah refinery, which is located in the area of Al – Qayyarah town toward the south east direction of Mosul city / Iraq. For this purpose, monthly samples were collected for five months from November 2013 to February 2014. Physical, chemical and biological tests were carried out on the samples including Electrical Conductivity, Total Dissolved Solid, Turbidity, Hardness, pH, Sulphate, Sodium and Potassium ions, Heavy metals, Oil,Chemical Oxygen Demandand the Total number of bacteria. The results of this study showed that there was clear variations in the values of those variables before and after treatment,such that values of the acidic function before treatment ranged between (7-8.1) compared with the value after treatment which ranged between (6.9-8.2).the values of Electrical Conductivity was (460-720)µmhos/cm before treatment while the values after treatment was(350-630)µmhos/cm the rate of total hardness before treatment was (233.8) mg/L compared with it’s rate after treatment (238.6) mg/L the nitrates ranged between(0.403-1.341)mg/L before treatment and (0.470-1.423) mg/L after treatment and for sulphate the values ranged between (56.16-67.416) mg/L before treatment compared with values after treatment which was (55.33-69.83) mg/L, the values of concentration for the heavy metals(Pb, Co, Cd, Cu) before treatment was (1.536-1.627), (0.05793-0.06644), (0.04794-0.04821), (0.5378-0.5733) mg/L and thevalues after treatment was (1.324-1.410), (0.06899-0.07814), (0.04845-0.06227), (0.5623-0.5825) mg/L and the total number of bacteria was between (100-1100) cell/ ml before treatment comparedwithresults after treatment (300-3000) cell/ml. The results show that the station’s pollutants removal was not efficient.