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تحضيـروتشخيص مركبات مقلدة للانسولين == SYNTHESIS AND CHARACTERIZATION OF INSULIN - MIMETIC COMPOUNDS

Author name: عمار جهاد صادق العبدلي
Supervisor name: اياد حمزة جاسم
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
Language: English
University location: Baghdad
First pages:
Abstract: تهيئ الكيمياء اللاعضوية مجالا خصبا لتصميم وتحضير مركبات صيدلانية لمعالجة الامراض العسيرة المعالجة في الوقت الحالي.منذ فترة طويلة استخدمت الادوية الفلزية لعلاج واعادة وظيفة فسلجة الجسم الى حالتها الاولية.ان عنصري الفناديوم والكروم يقدمان حالة مدهشة من بين العناصر الانتقالية حيث لها سلطة وصفة كيموفيزيائية نكشف من خلالها صفة مهمة كمقلدات لعمل الانسولين. ولهذا تم دراستها جيدا في علاج مرض السكري للنوع الاول والثاني.ان تصميم الادوية الفلزية في بحثنا يقيم بالدرجة الاولى بالتشابه الفراغي للاعمال السابقة والتركيب المبسط وصفة التواجد البايولوجي والذوبانية والامتصاصية.تم تحضير اربعة مركبات مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون ثمانية معقدات مختلفة تم اختيار ستة احماض امينية مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون اثنا عشر معقد مختلف تم اختيار الماركبتو حامض الخليك وحامض المانديلك للتاصر مع فلزات VO (II) وCr (III) الايونية لتكوين اربع معقدات مختلفة.تم اختيار خمسة سكريات مختلفة لتتاصر مع فلزات VO (II) وCr (III) الايونية لتكون عشرة معقدات مختلفة.تم عزل وتشخيص عدد من المركبات المختلفة عن طريق دراسة صفاتها الكيموفيزيائية بواسطة تحليل المعادن وتحليل عناصر C.H.N.S، واطياف التردد والانتقالات الالكترونية، والصفات التوصيلية والمغناطيسية، بالاضافة الى دراسة اطياف الرنين المغناطيسي النووي للهيدروجين.تمت دراسة تكوين بعض المعقدات في المحلول باتباع طريقة النسبة المولارية mole ratio.ان نتائج الدراسات في الحالة الصلبة والسائلة اعطتنا نتائج متطابقة. | Biomedical inorganic chemistry offers the potential for the design novel therapeutic agents for the treatment of diseases, which are currently intractable. Therapeutic metalodrugs have since long been employed to restore human physiology. Vanadium and chromium presents an outstanding case of a transition elements, the omnipotent physicochemical properties of which have unearthed it’s potential use as a serious insulin mimtic agents, well suited in the treatment of the heterogeneous disease of diabetes mellitus types I and II.The design of such metallodrugs has been at the fore front of the research depending on analogy of the previous work, simple structure, bioavailability, solubility and absorption property.Four different analog ligands have been synthesized to coordinate with VO (II) and Cr (III) metal ions to produce eight different complexes.Six different amino acids have chosen to coordinate with VO (II) and Cr (III) metal ions to produce twelve different complexes.Marcapto acetic acid and mandelic acid are also chosen to coordinate with VO (II) and Cr (III) metal ions to produce four different complexes.Five different sugars have been chosen to coordinate with VO (II) and Cr (III) metal ions to produce ten different complexes.Several of the synthesized compounds were isolated and characterized by studying their physicochemical properties such as C.H.N.S and metal analysis, vibrational and electric spsectra, conductivity, magnetic properties, in addition to 1H.N.M.R spectral study for some complexes.The formation of some of the complexes were studied in solution following the mole ratio method. The results of both solid state and solution studies gave identical results.

التقدير الطيفي لايون النحاس بوساطة الطريقة المباشرة وغير المباشرة بنقطة الغيمة باستخدام الحامض الامينيي الميثيونين == Spectrophotometric Determination of Copper Ion by Direct Method and Indirect Cloud Point Using the Amino Acid Methionine

Author name: اسماء نهاد زكي
Supervisor name: رافع قدوري عطيوي | سمية محمد عباس
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Baghdad
Language: English
University location: Baghdad
First pages:
Abstract: تشمل هذه الدراسة طريقتين مهمتين في التطبيق التحليلي لتعيين وفصل واغناء ايون النحاس الثنائي بطريقة نقطة الغيمة والطريقة الطيفية وذلك باستخدام مطياف الاشعة الفوق البنفسجية - المرئية. في الجزء الاول : تم استخدام الحامض الاميني الميثونين ككاشف تحليلي الذي يشكل مركب مخلبي مع ايون النحاس في الطور المائي وبدرجة حموضة محددة, والذي تكون له اعظم امتصاصية عند طول موجي (244 نانوميتر) لمعقد النحاس - الميثونين ضد الميثونين كبلانك.وتم دراسة الظروف الفضلى للتفاعل بالاضافة الى العوامل التحليلية الاخرى وافضل نتائج تم الحصول عليها لمنحني المعايرة والبيانات الاحصائية تحت الظروف الفضلى التي تم الحصول عليها بالطريقة الطيفية المباشرة لكميات صغيرة من النحاس, يطاوع قانون لامبرت بير في مدى تراكيز (0,1 - 10) ميكروغرام/مل مع امتصاصية مولارية (5842 لتر.مول - 1.سم - 1) وحد الكشف (0,0238 ميكروغرام/مل) في هذه الدراسة لوحظ حدوث تداخلات بعض المعادن مثل النيكل (II)والكروم(III) في ايون النحاس وقد تجاوزت الحد المسموح للتداخل , لذلك تم تطبيق الطريقة المقترحة بنجاح لتحديد ايون النحاس في عينات مختلفة من المياه.اما الجزء الثاني من الدراسة تستند على تكوين معقد كاره للماء بين ايون النحاس والميثونين الغنية بالترايتون 100 - X من خلال منهجية الاستخلاص بنقطة الغيمة الى جانب القياس الطيفي للاشعة فوق البنفسجية - المرئية, في هذه الطريقة يتشارك ايون الفلز مع الحامض الاميني الميثونين في تفاعل لتشكيل معقد مخلبي كاره للماء ويتم استخلاص هذا المعقد في درجة حموضة معينة عن طريق الاستخلاص بنقطة الغيمة باستخدام المركب السطحي غير الايوني ترايتون 100 - X كوسيط للاستخلاص.الطور العضوي الغني بالمادة السطحية يتم اذابتها باضافة الميثانول ويتم قياس المعقد طيفيا عند طول موجي (294 نانوميتر) لتحسين العوامل التي تؤثر على كفاءة استخلاص ايون النحاس باستخدام احد عوامل التحليلية وتشمل هذه العوامل درجة حموضة المحلول تركيز الليكند والمادة السطحية, درجة الحرارة والوقت التي تم تحديدها بالاضافة الى الكتيونات التي تعتبر متداخلات في ظل الظروف المثلى للتفاعل وقد تحقق عامل اغناء النحاس وكان منحني المعايرة الخطي (0,1 - 4) ميكروغرام/مل, حد الكشف والحد الكمي (0,0071) (0,0215) على التوالي. وتم مقارنة الطريقة المقترحة مع الطريقة الطيفية المباشرة لتعيين ايون النحاس ومن خلال النتائج المعروضة نلاحظ اختلافات كبيرة في الدقة والتوافق في الطريقتين وان الاستخلاص بنقطة الغيمة هي الاكثر دقة وتوافقية. تم تطبيق هذه الطريقة في عينات المياه. في هذه الدراسة تم تعيين تكافؤية المعقد عن طريق النسب المولية, التغيرات المستمرة (طريقة جوب) في درجة حموضة معينة واظهرت النتائج ان نسبة التكافؤ بين ايون النحاس الميثيونين هي 1 : 2. | This study in whole comprises two significant approaches in analytical application for direct determination and separation with preconcentration of copper ion by cloud point extraction methodology coupled with UV - Visible spectrophotometry.In the first part : The amino acid methionine was used as a chelating agent to form a complex with copper ion in aqueous phase at specific pH, which exhibits maximum absorption at (max= 244nm) against reagent blank. The optimum reaction conditions and other analytical parameters were evaluated. The results showed better optical characteristics for calibration curve and statistical data were obtained under optimum conditions using direct Spectrophotometric determination of micro amounts of copper ion. “Beer's law” is obeyed in the concentration range (0.1 - 10)g.mL - 1 , having molar absorptivity of 5842L. mol - 1. cm - 1. The value of detection limit was 0.0238g.mL - 1 . Interference study indicated that some metal ions like Ni+2, Cr+3 have exceeded the allowable limits of interference for copper ion absorbance signal. The proposed method was applied successfully for the determination of copper ion in various water samples.Part Two : Deals with the formation of a hydrophobic complex between copper ion and methionine in rich - surfactant phase, by “cloud point extraction” (CPE) methodology, coupled with UV - Visible spectrophotometry. This method involved reaction of copper ion with methionine as a chelating agent to form a hydrophobic complex. Which was extracted at specific pH by CPE technique using nonionic surfactant Triton X - 100.as an extraction medium. The complex was surrounded by surfactant micelles. The surfactant - rich phase was diluted with methanol and the complex was measured spectrophotometrically at it's (max= 294nm). Different factors that can influence the extraction efficiency of copper ion has been optimized by using one - factor - at - a - time (OFAT). These factors include solution pH, reagent and surfactant concentrations, temperature and incubation time. Besides the interference effect of cations was also considered under the optimized conditions, “preconcentration factor” of 90 was achieved. The linear range was (0.1 - 4)g.mL - 1 with “limit of detection” and limit of quantification (0.0071), (0.0215)g.mL - 1 respectively and molar absorptivity of (19621.5) L. mol - 1. cm - 1.The Stoichiometric study was determined by “mole ratio method and continuous variation method” (Job's) at specific pH. The results showed that the Stoichiometric ratio between copper ion and methionine was 1 : 2.The proposed method is compared with the direct spectrophotometry determination of copper ion and the results have shown that there is a significant differences in accuracy and precision between the two methods and the cloud point extraction which indicates that the latter is more accurate and more precise. The suggested method was applied successfully for the determination of copper ion in water samples

تحضير ايمايدات حلقية ثنائية وبعض مشتقاتها الكبريتية ودراسة خواصها الطيفية والتركيبية , عمليا ونظريا باستخدام نظرية دالية الكثافة == IR, NMR, MS Spectra and Structure of Some prepared Bicyclic Imides and Their Thione Derivatives; Experimental and Density Functional Theory studies

Author name: عادل امعلا ضمد ال ازيرج
Supervisor name: ناجي علي عبود
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
Language: English
University location: Basrah
First pages:
Abstract: The present work involved four parts : First step concerned with the preparation some N, N’ - alkyl (aryl) bismaleimic acidsvia reaction of twice molar amounts of maleic anhydride and hydrazine for compound(A1), and different alkyl and aryl - diamines for compounds A2 - A7. The reaction wascarried out via nucleophilic attack of amino group in maleic anhydride. The structureof the compound (2Z,2Z’) - 4,4’ - (ethane - 1,2 - diylbis (azanediyl)) bis (4 - oxobut - 2 - enoicacid) (A2) was also unambiguously confirmed by X - ray single crystal structureanalysis. The white crystal crystallizes in the monoclinic system, space group C2/cwith the cell dimensions a =7.108(3), b=7.370(2), c= 20.859(6) Å, β = 91.260(4)oand Volume = 1092.65(6) Å3.Molecule is stabilized by an intramolecular O—H…O hydrogen bond. In thecrystal, molecules are connected through intermolecular N—H…O hydrogen bonds.Intermolecular and intramolecular hydrogen bonds coexist to stabilize the structure.The geometry calculated of compounds A1 - A7 was optimized using a Densityfunctional theory DFT with B3LYP hybrid functional and 6 - 311G (d, p) basis set, andis in good agreement with the structure obtained by the X - ray single crystal structureof compound A2. Also the fundamental vibrational frequencies of vibrational bandswere evaluated.The second part of this study was the treatment of N,N - alkyl and (aryl)bismaleimic acid (A1 - A7) with suitable dehydrating agents lead to dehydration andcyclization producing the corresponding N,N - alkyl and (aryl) bismaleimide (AD1 - AD7).The structure of the compound 1,1’ - (sulfonylbis(4,1 - phenylene)) bis (1H - pyrrole - 2,5 - dithione) (AD7) was also unambiguously confirmed by X - ray single crystalstructure analysis. The colorless crystal crystallizes in the monoclinic system, spaceAbstractix0200040000CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2CH2phenyl4,4' - sulfonyldianilinedirect Aliphatic AromaticWavenumber cm¯¹Types of RCH str.CH2 - N strC=O strC - Ngroup P21/c with the cell dimension a =11.698(3), b=15.002(3), c= 20.053(6)Å andβ = 98.818(2)o Volume = 3478.07(13) Å3.FT - IR spectra show the position of the absorption bands vary with the type andlength of the link spacer (R) between the two maleimide rings on the compoundsAD1 - AD7.The absorption frequency of vinyl group increases with increasing methylene aliphatic chain spacer link between two maleimides ring, the correlation between some absorption bands and the type (direct link or aliphatic or aromatic) and length of aliphatic chain link spacer (R) between the two maleimide rings in the studied compounds AD1 - AD7 shown in the chart below.In the third part, a series of new bisthimalemide derivatives were prepared by thionation the compounds AD3, AD6 and AD7 with Lawesson’s reagent LR. Subsequent reaction of bismaleimimides AD3, AD6 and AD7 with Lawesson’s reagent afforded dithio derivatives.

التشخيص الكيميائي والفولتامتري للبولي بيوتيلين سكسنيت الملدن بواسطة ايبوكسي (زيت النخيل)

Author name: حسن رحيم حمود الدحيدحاوي
Supervisor name: عماد عباس جعفر | هناء عداي علي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: في هذه الدراسة ، تم استخدم ايبوكسيي زيت النخيل EPO كملدن للبولي بوتيلين سكسينيت باستخدام الكلوروفورم كمذيب ، تم خلط ستة اوزان من PSPE وقد استخدم جهاز FTIR الطيفي لتحديد المجاميع الفعالة . كما وتم قياس الاستقرارية الحرارية والتحلل البيولوجي ، والخصائص المورفولوجية للخليط بواسطة جهاز التحليل الحراري الوزني TGA ، المجهر الالكتروني الماسح SEM وتقنية FTIR ، حيث اظهرت النتائج بان هناك بعض التاثر بين المركبين بوجود الاواصر الهيدروجينية التي تربط بين نهايات المجاميع الفعالة للبوليمر OH وبين حلقة الايبوكسي . مزيج الـ PSPE اظهر استقرار حراري عالي وتحسن في الخواص البيولوجية مقارنة مع الـ PBS النقي . كما اظهرت النتائج المورفولوجية للخليط ان EPO كان ذو قابلية امتزاجية جيدة مع PBS. تم تعديل قطب الكربون الزجاجي GCE مع طبقه رقيقة من (PSEP ) باستخدام طريقة محلول التبخر لانتاج القطب الجديد المعدل . PSEP/GC تم ايضا دراسة عمليات الاكسدة والاختزال لسداسي سيانيد الحديدات (II) باستخدام الـCyclic Voltammetry . وقد تبين ان ذروة الفصل ΔEpa - c ) ) بين قمم الاكسدة لايون فروسيانيد في محلول مائي هو 120 ملي فولت ، ونسبة التيار لقمم الاكسدة، IPA / IPC، كانت 1.6 لـ PSEP / GCE، مؤشرا انعكاسية وقابلية توصيلية جيدة للقطب المعدل. وبالتالي، فانه يمكن استخدامها لتحليل الجهد الكهروكيميائي . الخواص الفيزيائية للقطب المعدل PSEP / GCE تمثلت بالصلابة الجيدة، التصاق العالي على الاسطح المعدنية للقطب الالكتروليت الجامع ، بالاضافة الى الذوبانية والاستقرارية الجيدة للـPSEP على .GCE ايضا، الحساسية في ظل ظروف الـ cyclic voltammetry تعتمد بشكل كبير على تراكيز مختلفة من فروسيانيد ، الالكتروليت المستخدم ومعدل المسح . وقد لوحظ خلال معدلات مسح مختلفة بان قمم الاكسدة والاختزال للحديد / (III) الحديد (II) تمت بعملية معكوسة. | In this study, epoxidized palm oil (EPO) was utilized as a blended for poly butylene succinate (PBS) using chloroform as a solvent by solution casting process at six weight of PSEP. Fourier - transform infrared (FTIR) spectroscopy was used to identify the functional groups of PBS and PSEP blends. Thermal stability, biodegradable, and morphological properties of the blends were investigated by thermo gravimetric analyzer (TGA), and scanning electron microscope (SEM) technique. The FTIR spectra indicate that there are some molecular interactions by intra molecular hydrogen bond between PBS and EPO. All sets of PSEP blends show high thermal stability and significant improvement of biodegradable properties compared to pure PBS. Morphological results of PSEP blends show that EPO was good miscible with PBS. Aglassy carbon electrode (GCE) was modified with a poly butylene succinate - epoxidized palm oil (PSEP) film using a solution evaporation method to produce a new modified electrode PSEP/GCE. The redox process of K4[Fe(CN)6] during cyclic voltammetry was studied using the PSEP/GCE. It was found that the peak separation (∆Epa - c) between the redox peaks of ferrous cyanide ion in an aqueous solution is 120 mV and the current ratio of redox peaks, (Ipa/Ipc), is 1.6 for the PSEP /GCE, indicating good reversibility with good conductivity of the modified electrode. Hence, it can be used for voltammetric analysis. The physical properties of the modified electrode PSEP/GCE include good hardness, high adhesion to the metal surfaces of electrode collectors, solubility and good stability of the PSEP on GCE. Also, the sensitivity under conditions of cyclic voltammetry is significantly dependent on different concentrations of ferrous cyanide , the electrolyte used and the scan rate. At different scan rates, oxidation - reduction peaks of Fe(III)/Fe(II) were observed in a reversible process

تحضير عوامل مساعدة من بعض اكاسيد الفلزات وتطبيقاتها في الاكسدة الحرارية والضوئية == Preparationof Catalysts From Several Metals Oxides and their Application in Thermal and PhotoOxidation

Author name: فاطمة علاوي عبد السجاد
Supervisor name: موسى عمران كاظم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:

دراسة الاطياف الاهتزازية والفعالية البايولوجية لبعض القلويدات == A study of the vibrational spectra and the biological activity of some alkaloids

Author name: ايمان عبد الوهاب عبد الله الكويتي
Supervisor name: عبد الرزاق عبد الجليل العيسى | حسين عبد الكاظم عبد الحسين
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: The present study was conducted to extracts several alkaloids and their potency on the contraction of smooth’s Rat intestine .to achieve these aims : (Okra, Potato, Cilca ,Pomegranate, Sweet melon, Water melon, Eggplant , pumpkin , Quince , Oaks, Apple, Broad been ,Cauliflower ,Cinnamon ,spinach) were subjected to extraction by petroleum ether and ethanol.HPLC and Mayer’s test revealed significant amounts of pelletierin from punica granatum,lupanine from spinacia oleracea,sinaxalen from brassica oleracea,jasmonoyl tyrosine alkaloid from vica faba ,solanidine from solanum tuberosum and solanine from solanum melongena,in the enrolled plants.The amounts of these alkaloids were (0.22,0.015,0.043,0.036,0.041,0.031) mg/g Respectively .The interaction of alkaloids (0.1) g/L and the contraction of smooth muscle in rat was examined by IR spectroscopy. with the data exhibited stretching band of (C - N) bond in the rang of (1215 - 1020),as described in the literatures .The wave number of the stretching bands of (C - N)in alkaloids were found to be inversely proportional with the molecular weight of alkaloids .Alkaloids were found to elicit Rat intestinal strain according to the order Pelletierine>Lupanine>Sinaxalen>Jasmonoyltyrosine> Solanidine>Solanine.These results suggest the involvement of (C - N) bonds in alkaloids during the induction of smooth muscle contraction.

دراسة العوامل الكيميوحيوية والتنميط الجيني للانزيم المحول للانجيوسين لدى مرضى اعتلال الكلية السكري النوع 2 == Biochemical Study and Angiotensin converting enzyme polymorphism of Nephropathy in T2DM Patients

Author name: زينب عباس جواد الطالبي
Supervisor name: حيدر كامل زيدان السعدي | محمود حسين هدوان
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: Diabetes is characterized by high levels of blood - glucose resulting from defect insulin hormone secretion or insulin action, or both of them. Chronic high blood - sugar lead to development and failure in many organs in the body such as heart, blood vessels of the eyes, nerves system and kidneys.The Study evaluation of Angiotensin Converting Enzyme - 1 and Angiotensinogen in Type 2 Diabetic patients according to the following steps : it is directed to evaluate Biochemical parameters in type 2 diabetic patients. Measure the levels of some hormones and some parameters. Study the relationships between these hormones and the Biochemical parameters. The association of Angiotensin converting enzyme gene in some hormonal and physiological parameters in type 2 diabetic Iraqi patients. Determined by Polymerase Chain Reaction (PCR). while the hormones including (Insulin and Erythropoietin) and the physiological parameters (insulin resistance, insulin sensitivity, Fasting Blood Glucose; HbA1C; microalbuminuria; systolic and diastolic blood pressure).This case - control study was done in a period of March 2016 to May 2016, from Al - Sadder Medical City in Al - Najaf center for Diabetes and Endocrine. All blood samples of patients were collected in fasting (8 - 10hr.) Number of patients in Diabetes mellitus (DM) type II. Total patients were (n=66), then divided into three groups according to the duration of the disease, the First subgroup (less than 5 years) (n=22), Second subgroup (5 - 10 years) (n=22) and the last subgroup more than 10 years (n=22). The healthy control includes (n=22) subjects, total numbers becomes (88 persons).VISummaryExcluded from this study : Type I diabetes, Females, smokers Patients, random Patient uncontrolled hypertension, alcoholic patients, types of cancer, Hepatitis and Removal of glands. Both groups were subjected to full history including age, BMI, complete clinical examination such as blood pressure measurement. Laboratory measurements including, fasting blood sugar, HbA1C, Microalbuminuria, Insulin hormone, Erythropoietin hormone, Estimation insulinresistance and sensitivity, Extraction DNA from frozen blood for all control and patients then, determination of ACE I/D genotype were done by using PCR technique.The results show significantly Elevation in Microalbuminuria, HbA1c , Fasting blood - sugar, and insulin resistance in nephropathy diabetic type 2 patients compared with healthy control.ACE - 1 enzyme levels have significant increase and lead to the hypertension in the Diabetic patients. There is no relationship between Erythropoietin hormone level and blood pressure deduce that EPO did not raise blood pressure with the patients according to the results of this study, but caused from Angiotensin converting enzyme - 1. The frequency of DD genotype was 21/44 (50%) in patients type 2 more frequent and significant that was significantly higher than that of patient group ID and II with P value =0.036. while there was no significant in ID genotype between patients in group ID 14/44(31%) with p=0.92 and patient in group II genotype 9/44 (20%) with P value=0.07.This study found that DD genotype of ACE gene may be associated with development of diabetic nephropathy among Iraqi patients and this could lead to the prevention and treatment of this complication (Diabetic nephropathy) in Iraqi diabetic patients.

التقدير الطيفي للنايترازيبام وهيدروكلوريد الكلوربرومازين في بعض المستحضرات الصيدلانية باستخدام تفاعلات لونية جديدة == Spectrophotometric Determination of Nitrazepam and Cloropromazine - HCl in some Pharmaceutical Formulations using a new Colorimetric reactions

Author name: سارة محمد علي المطيري
Supervisor name: قاسم حسن كاظم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: الفصل الاول : تضمن مقدمة عامة عن الادوية والتحاليل الدوائية وبعض المفاهيم الاساسية عن التحليل بالطرق الطيفية المعتمدة على امتصاص الاشعة فوق البنفسجية والمرئية المستعملة في هذا النوع من التحاليل, حيث تضمن البحث على مقدمة عامة عن تفاعلات الازوتة - الاقتران واهميتها في التقدير الطيفي للعديد من المركبات الدوائية, وايضا التفاعلات الخاصة باملاح الدايزونيوم. ومقدمة عن تفاعلات قواعد شف وميكانيكية حدوث هذه التفاعلات, بالاضافة الى تصنيف لقواعد شف حسب المجاميع المانحة. ومقدمه عامة عن دواء النايترازيبام واستعراض للطرق التحليلية المستعملة في تقديره. تضمن البحث ايضا على مقدمة عامة عن تفاعلات الاقتران التاكسدي واهميته في التقدير الطيفي للعديد من المركبات الدوائية واهم العوامل المؤثرة فيها واهم الميكانيكيات المتبعة في هذه التفاعلات. ومقدمة عامة عن مركبات الفينوثايزين وعرضا موجزا لبعض الخواص الكيميائية والاستعمالات الطبية والصيدلانية لمركب الفينوثايزين المدروس هيدروكلوريد الكلوربرومازين (CPZ), واستعراض موجز للطرائق التحليلية المستخدمة في تقدير هذا الدواء.الفصل الثاني : تضمن وصف للاجهزة المستخدمة في الطريقة والمقترحة وكذلك المواد الكيميائية المستخدمة والشركات المصنعة لها, بالاضافة الى طرق تحضير محاليل الادوية والكواشف والحوامض والقواعد والعوامل المؤكسدة والمستحضرات الصيدلانية, بالاضافة الى الطرق القياسية للادوية المستخدمة في الدراسةالفصل الثالث : تضمن وصف طريقتين طيفيتين بسيطة وحساسة لتقدير النايترازيبام في المحلول المائي بعد اختزال مجموعة النايترو (NO2 - ) الموجودة فيه الى مجموعة امين (NH2 - ) باستخدام الزنك وفي الوسط الحامضي, في حالته النقية وفي بعض مستحضراته الصيدلانية, حيث اعتمدت الطريقة الاولى على اقتران النايترازيبام المختزل مع الكاشف العضوي (الثايمول) في الوسط القاعدي, واعطائه صبغة ازو برتقالية مستقرة وذائبة في الماء لها اقصى امتصاص في الطول الموجي (477) نانوميتر. وجد ان الطريقة تتبع قانون بيــر لامبـــرت بمدى تركيز (12 - 0.1) مايكروغرام. مل 1 - , وبمعامل امتصاص مولاري (104×(2.264 لتر.مول1 - .سم1 - , وحساسية ساندل (0.0124) مايكروغرام. سم2 - , وحد كشف (0.02) مايكروغرام. مل1 - , وحد التقدير الكمي (0.072) مايكروغرام. مل 1 - , ومعدل نسبة استرداد (99.52)% , ومعدل الانحراف القياسي النسبي (0.7323)%. اما الطريقة الثانية فاعتمدت على اقتران النايترازيبام المختزل مع الكاشف (بارا - هيدروكسي بنزالدهايد) ليعطي قاعدة شف برتقالية اللون مستقرة وذائبة في الماء لها اقصى امتصاص عند الطول الموجي (484) نانوميتر. وجد ان الطريقة تتبع قانون بيــر لامبـــرت بمدى تركيز (10 - 0.1) مايكروغرام. مل 1 - , وبمعامل امتصاص مولاري (104×(3.14 لتر.مول1 - .سم1 - , وحساسية ساندل (0.0089) مايكروغرام. سم2 - , وحد كشف (0.029) مايكروغرام. مل1 - , وحد التقدير الكمي (0.098) مايكروغرام. مل 1 - , ومعدل نسبة استرداد (99.9)% , ومعدل الانحراف القياسي النسبي (0.579)%. طبقت الطريقتين بنجاح لتقدير النايترازيبام المختزل في المستحضر الصيدلاني والذي كان عبارة عن (حبوب) , اذ وجد ان نتائج الطريقتين تتفق مع المحتوى الاصلي للمستحضرات الصيدلانية ومع نتائج الطريقة القياسية المستعملة في تقدير النايترازيبام, وتم تقييم نتائج الطريقتين المقترحتين من خلال حساب قيم اختباري t وF والتي كانت اقل من القيم الجدولية عند مستوى الثقة 95% مما يدل على ان الطرق المقترحة والطريقة القياسية لا تختلفان بشكل ملحوظ في الدقة والتوافقية. ايضا تضمن الفصل وصف طريقة طيفيه بسيطة وحساسة لتقدير هيدروكلوريد الكلوربرومازين (CPZ) في المحلول المائي بحالته النقية وفي مستحضراته الصيدلانية , تعتمد هذه الطريقة على الاقتران التاكسدي بين الدواء والكاشف العضوي (2,5 - Dimethoxyaniline) واعطاء صبغة زرقاء مستقرة وذائبة في الماء لها اقصى امتصاص عند الطول الموجي (717) نانوميتر. وجد ان الطريقة تتبع قانون بيــر لامبـــرت بمدى تركيز (14 - 0.05) مايكروغرام. مل 1 - , وبمعامل امتصاص مولاري (104×(4.04 لتر.مول1 - .سم1 - , وحساسية ساندل (0.0087) مايكروغرام. سم2 - , وحد كشف (0.024) مايكروغرام. مل1 - , وحد التقدير الكمي (0.082) مايكروغرام. مل 1 - , ومعدل نسبة استرداد (99.94)% , ومعدل الانحراف القياسي النسبي (0.149)%. طبقت الطريقة بنجاح لتقدير هيدروكلوريد الكلوربرومازين في المستحضر الصيدلاني والذي كان عبارة عن (حبوب) , اذ وجد ان نتائج الطريقة تتفق مع المحتوى الاصلي للمستحضرات الصيدلانية ومع نتائج الطريقة القياسية المستعملة في تقدير هيدروكلوريد الكلوربرومازين, وتم تقييم نتائج الطريقة المقترحة من خلال حساب قيم اختباري t وF والتي كانت اقل من القيم الجدولية عند مستوى الثقة 95% مما يدل على ان الطرق المقترحة والطريقة القياسية لا تختلفان بشكل ملحوظ في الدقة والتوافقية. | First chapter includes a general introduction on drugs, pharmaceutical analysis and some basic concepts, based on absorption of ultraviolet and visible light that used in this type of analysis. It had included an introduction to the diazo coupling reaction and its importance in spectrophotometric estimation of many pharmaceutical compounds, as well as the most important factors affecting on the stability. Also include general introduction on Schiff base reactions, the mechanism of this reaction, classification of Schiff base according to the donor groups, general introduction about Nitrazepam (NZP) drug and review of the analytical methods that have been used for the determination of Nitrazepam. Also general introduction about oxidative coupling reaction and its importance in spectrometric determination of many pharmaceutical compounds. Also, the most important mechanisms. General introduction about Chlorpromazine - Hydrochloride (CPZ) drug and review of the analytical methods that have been used for the determination of (CPZ). Second chapter : describes the instruments that have been used in this study, preparation of drugs solutions and their pharmaceutical formulations, also acids, bases and oxidizing agents solutions. And describs the standard methods of these drugs. Third chapter : describes two simple and sensitive methods for the determination of reduced nitrazepam (NZP) in aqueous solution, in its pure state and in pharmaceutical preparations after reducing nitro group ( - NO2) to the amine group ( - NH2) . The first method based on the coupling of reduced (NZP) with organic reagent (Thymol) in alkaline medium to give a stable orange azo - dye soluble in water that has maximum absorption at wavelength (477) nm.Beer's law was obeyed between (0.1 - 12) µg.ml - 1 , a molar absorptivity (2.264 * 104) L.mol - 1.cm - 1 , Sandal's sensitivity (0.0124) µg.ml - 2, the LOD was (0.02) µg.ml - 1 , LOQ was (0.072) µg.ml - 1 , average recovery was 99.52 %, and the average of relative standard deviation was 0.7323 %. The second method depends on coupling of reduced (NZP) with the organic reagent (p - Hydroxybenzaldehyde) to form orange Schiff base soluble in water that has maximum absorption at wavelength (484) nm.Beer's law was obeyed between (0.1 - 10) µg.ml - 1 , a molar absorptivity (3.14 * 104) L.mol - 1.cm - 1 , Sandal's sensitivity (0.0089) µg.ml - 2, the LOD was (0.029) µg.ml - 1 , LOQ was (0.098) µg.ml - 1 , average recovery was 99.9 %, and the average of relative standard deviation was 0.579 %. These two methods were applied successfully for the determination of reduced (NZP) in pharmaceutical formulations (tablets), the analytical results were compared with the claim content of pharmaceuticals and also with the standard method was used for determination of nitrazepam, evaluating the proposed methods results by using F and t - test. It was found results experimental F and t value at 95% confidence level did not exceed the critical values. This means the proposed methods do not differ significally in accuracy and validity with standard method. Also, this chapter described a simple and sensitive spectrophotometric method for determination of chlorpromazine hydrochloride (CPZ) based on oxidative coupling reaction between (CPZ) and the reagent (2,5 - dimethoxyaniline) in the presence of oxidizing agent and acidic medium, to form blue complex soluble in water that has maximum absorption at wavelength (717) nm.Beer's law was obeyed between (0.05 - 14) µg.ml - 1 , a molar absorptivity (4.04 * 104) L.mol - 1.cm - 1 , Sandal's sensitivity (0.0087) µg.ml - 2, the LOD was (0.024) µg.ml - 1 , LOQ was (0.082) µg.ml - 1 , average recovery was 99.94 %, and the average of relative standard deviation was 0.149 %. This method was applied successfully for the determination of (CPZ) in pharmaceutical formulations (tablets and injection), the analytical results were compared with the claimed content of pharmaceuticals and also with the standard method was used for determination of (CPZ), evaluating the proposed method results by using F and t - test. It was found results experimental F and t value at 95% confidence level did not exceed the critical values. This means the proposed method do not differ significally in accuracy and validity with standard method

تحضير وتشخيص المركبات النانوية Nb2O5 /CdS ودراسة الامتزاز وفعالية المحفز الضوئي للايونات الفلزية الانتقالية == Synthesis, Characterization of Nb2O5 /CdS Nano Composites, and Study Sorption and Photocatalytic Activity of Transition Metal Ions

Author name: زينة طالب عمران
Supervisor name: ندى يحيى فيروز
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: This study includes preparation of nano composite catalyst Nb2O5\CdS at various ratios by using wet commixing method with changed calcination temperature 200, 500 and 800 ⁰C .The catalysts were characterized using X - rays diffraction (XRD), Fourier Transform Infrared (FTIR), Scanning Electron Microscopy SEM and Atomic Force Microscopy (AFM). Then used all of these ratio that calcinated at various temperature in degradation procedure of both Co (II) and Cu (II) from their aqueous solutions. It was found that the catalyst with a ratio of ( 0.85 : 0.15) and (0.75 : 0.25), which was calcinated at 800⁰C it’s the best ratios for Co(II) and Cu(II). Removal of Co (II) was examined after optimization of removal conditions, for example, mass of catalyst , pH of mixture, effect of temperature ,effect of concentration of Co (II) and effect of addition hydrogen peroxide . The best conditions for this case were pH=4, 0.1 g , 500ppm and temperature equal to30ºC, 0.1M of H2O2. Activation energy was calculated using Arrhenius plot and it was 26.28 kJ/mol.Study adsorption of Co(II) was examined after ideal of conditions for example effect of mass of catalyst , effect of concentration of Co (II), pH of mixture, effect of temperature . The ideal conditions for this case were 0.1 g , 500ppm , temperature equal to30ºC, pH=4, and. Activation energy was calculated using Arrhenius plot and it was 8.363 kJ.mol - 1Kinetics of this procedure was investigated and it was fitted with the pseudo first order kinetics. In addition to that, adsorption isotherms for this process were applied for both Langmuir and Freundlich adsorption isotherms. The obtained results presented that it was agreedIIwith Freundlich adsorption model. Study thermodynamic parameters results exhibited that the negative values of ΔG( - 2.346, - 3.571 , - 4.697 , - 5.259 kJ/mol ) for temperature (15 ,20 ,23 ,30 )oC and the positive ΔH (+55.66kJ/mol) and ΔS (+0.201kJ/mol K) .Removal of Cu (II) was examined after ideal conditions such as mass of catalyst , pH of mixture, effect of temperature , effect of concentration of Cu (II) and effect of addition hydrogen peroxide . The ideal conditions for this case were 0.05 g, 500ppm, 30ºC , pH=3 ,0.1M of H2O2. Activation energy was calculated using Arrhenius plot and it was 9.814 kJ.mol - 1.Study adsorption of Cu (II) was investigated after best of conditions for example effect mass of catalyst , effect of concentration of Co (II),pH of mixture, effect of temperature . The ideal conditions for this case were 0.15 g , 500ppm ,30ºC, and pH=3. Activation energy was calculated using Arrhenius plot and it was 8.866 kJ.mol - 1Kinetics of this process was studied and it was fitted with the pseudo first order kinetics. In addition to that, adsorption isotherms for this procedure were applied for both Langmuir and Freundlich adsorption isotherms. The obtained results presented that it was agreed with Freundlich adsorption model. Study thermodynamic parameters results exhibited that the negative values of ΔG( - 3.110, - 3.919, - 5.785 , - 8.300kJ/mol ) for temperature(15 ,20 ,23 ,30) oC and the positive ΔH (+58.42kJ/mol ) and ΔS (+0.213 kJ/mol K ) .

تصميم وحدة حقن جرياني جديدة لتقدير ايون اليوديد وايون الكرومات == Design new flow injection unit for the determination of iodide ion and chromate ion

Author name: زهير صالح عبيد الشافعي
Supervisor name: داخل ناصر طه الزركاني
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: he third chapter contains Several axis's is : The first axis is design FIA unit for determination of chromate ion , and of the work , their components and chosen the Optimum Design .* The second axis included study optimal conditions of system ( effect of flow rate , effect of reaction coil , sample loop , starch loop , calibration curve , reproducibility , dispersion coefficient , sampling rate and dead volume . after fixing the optimum conditions , detection limit ( 5 ppm ) , linearity was over the range of ( 10 ppm - 90 ppm ) and linearity coefficient ( R2 ) was ( 0.999 ) .* The three axis is using the same system in determination iodide ion after change the valve it was best results .* The four axis included study optimum conditions of new system ( effect of flow rate , effect of reaction coil , sample loop , starch loop , calibration curve , reproducibility , dispersion coefficient , sampling rate and dead volume . after fixing the optimum conditions , detection limit ( 3 ppm ) , linearity was over the range of ( 5 ppm - 70 ppm ) and linearity coefficient ( R2 ) was ( 0.9995 ) . also the study calibration curve of chromate in the new system , after fixing the optimum conditions , detection limit ( 3 ppm ) , linearity was over the range of ( 10 ppm - 90 ppm ) and linearity coefficient ( R2 ) was ( 0.998 ) .* The last axis included is study application on the tow system and the difference , system one been applied on aqueous solutions of chromate at ( 50 ppm , 70 ppm ) , system tow been applied on aqueous solution of chromate at ( 50 ppm , 70 ppm ) , Medicine chromium picolinate , aqueous solution of iodide at ( 15 ppm , 25 ppm ) and medicine Boviden iodid 4 %

تحقق نظري لاليات تفاعلات التحلل الضوئي لمركبات الهالوهيدروكربون في طبقة الستراتوسفير == Theoretical Investigation of Photolysis Reactions Mechanisms For Halo - Hydrocarbon Compounds In Stratospheric Layer

Author name: رؤى عبد الحسين عبد العباس المسعودي
Supervisor name: عباس عبد علي دريع الصالحي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: تم دراسة الية تفاعل نضوب الاوزون بتاثير ثلاث مركبات من هاليدات الهيدروكاربونات ( 1 - برومو - 1 - كلورو - 1,1 - ثنائي فلوروميثان و1 - كلورو - 2,2,2,1 - رباعي فلوروايثان و1,3 - ثنائي بروموبروبان) نظريا في الطور الغازي. حيث ان دراسة المحاكاة تضمنت مسالك تحلل ضوئي مختلفة. استخدمت مختلف طرائق الكم مثل الحسابات شبه التجريبية والحسابات الاساسية الاولية وحسابات نظرية دالة الكثافة. تم احتساب الفعالية الكيميائية والقيم الطاقية لجميع الاصناف الكيميائية التي شملتها الدراسة بواسطة سطوح جهد الطاقة ومعاملات الاواصر وعزوم ثنائية الاقطاب وطاقات الاوربيتالات الجزيئية وطاقة نقطة الصفر لاستبيان المسلك الاكثر احتمالا لتفاعلات التحلل الضوئي واقتراح ميكانيكية التفاعل. تم تقدير الدوال الثرموديناميكيه (∆S°, ∆G°, ∆H°) وطاقة التنشيط وثابت السرعة والتردد الخيالي مع نقطة الصفر لتقدير الحالة الانتقالية الحقيقية والاصناف الكيميائية الاكثر احتمالا بتفاعلات التحلل الضوئي والتي تشارك بميكانيكية نضوب الاوزون.وجد من خلال هذه الدراسة : - ان فجوة الطاقة بين الصيغ الكيميائية التركيبية للاوزون مساوية الى 33.195 كيلو سعره للمول الواحد مع اقل قيمة من حرارة التكوين للاوزون الزاوي والتي مقدارها 45.2773 كيلو سعره للمول الواحد لذلك ان صيغة الاوزون الزاوي (bent ozone) اكثر استقرارا من صيغة الاوزون الحلقي ويمكن ان تتفاعل مع هاليدات الهايدروكاربونات في توجهات فراغية مختلفة. يحصل تفاعل التحلل الضوئي لمركب بروموكلورو ثنائي فلوروميثان من خلال اصرة C - Br مع طاقة تنشيط مقدارها 46.954كيلو سعره للمول الواحد وانثالبي تفاعل مساوي الى 49.749 كيلو سعره للمول الواحد عند الظروف القياسية. تمت ميكانيكية استنزاف الاوزون بواسطة الجذور الحرة الكلور والبروم وثنائي فلوروميثل مع انثالبي تفاعل مقداره من - 48.99الى - 49.057 كيلو سعره للمول الواحد وثابت سرعه مساوي الى 5.34*1017, 6.914*1021 و7.43*1081 ثانيه - 1 لجذر البروم , الكلور وثنائي فلوروميثل على التوالي. ثلاث مولات من الاوزون استنزفت بواسطة مول واحد من مركب بروموكلورو ثنائي فلوروميثان. استنزاف الاوزون بواسطة 1 - كلورو - 2,2,2,1 - رباعي فلوروايثان يتم من خلال جذر الكلور عند طاقة ضوء مساوية الى 65.636 كيلو سعره للمول الواحد وطول موجي مقداره 407.8643 نانوميتر حيث ان مول واحد يستنزف ست مولات من الاوزون مع انثالبي تفاعل مساوي الى - 252.64 كيلو سعره للمول الواحد وطاقه حرة مقدارها - 291.376 كيلو سعره للمول الواحد.3,1 - ثنائي بروموبروبان يتفكك عند طول موجي مساوي الى 442.571 نانوميتر ليحرر جذر البروم وثلاثي بروموبروبان مع طاقة تنشيط مساوية الى 98.624 كيلو سعره للمول الواحد. الاصناف الفعالة الناتجة تستهلك الاوزون بمسالك تفاعل مختلفة لتعطي جذر الالكوكسي وواوكسيد البروم مع تكوين جزيء الاوكسجين بانثالبي تفاعل كلي مقداره - 157.9 كيلو سعره للمول الواحد. | Reaction mechanism study of ozone depletion has been carried out on three selected compounds of halo - hydrocarbons (1 - bromo - 1 - chloro - 1,1 - diflouromethane, 1 - Chloro - 1,2,2,2 - tetrafluoroethane, and 1,3 - dibromopropane) that’s achieved theoretically in the gas phase. The simulation study involves different photolysis reaction pathways. Different quantum methods such as semiempirical, Ab initio and density functional theory have been used in this study. The chemical reactivity and energetic properties of all chemical species that are involved in this study have been computed by the potential energy surface, bond parameters, dipoles moments, molecular orbital energies and zero point energy to estimate the most probable pathway of photolysis reaction to proposed the reaction mechanism. Thermodynamic functions (∆S°, ∆G°, ∆H°), activation energies, rate constant, the imaginary frequency with zero point energy to estimate the real transition state have been calculated to predict the most probable species through photolysis reactions that are contributing to ozone depletion mechanism. From this study, it is found that the energy gap between cyclic and bent ozone equal to 33.195 kCal mol - 1 and the lowest value of heat of formation of bent ozone which equal to 45.2773 kCal mol - 1 so, the bent ozone more stable than cyclic ozone and react with halo - hydrocarbons species in different orientations. The photolysis reaction of bromochlorodiflouromethane occurs through C - Br bond with an activation energy equal to 46.954 kCal mol - 1 and enthalpy change of reaction equal to 49.749 kCal mol - 1 at STP. The depletion mechanism is completed by bromine, chlorine and diflouromethyl radicals with enthalpy change of reaction fall in the range - (48.99 - 49.057) kCal mol - 1 and rate constant values for the reaction of these radicals with ozone equal to 5.34*1017, 6.914*1021, 7.43*1081 s - 1 for bromine, chlorine and diflouromethyl respectively, to deplete three moles of ozone by one mole of bromochlorodiflouromethane. Ozone depletion by 1 - Chloro - 1,2,2,2 - tetrafluoroethane occurs through chlorine radical at 65.636 kCal mol - 1(407.8643nm) of light energy where one mole of the compound destruct six moles of ozone with enthalpy change of reaction equal to - 252.64 kCal mol - 1, and free energy change equal to - 291.376 kCal mol - 1. 1,3 - dibromopropane breakdown at 442.571 nm of light wavelength to released bromine and 3 - bromopropane radicals with activation energy equal to 98.624 kCal mol - 1. 1,3 - dibromopropane exists in three isomers C2, C1 and C2V was found in this study that the isomer C2 is more stable with total energy being equal to - 26652.031 kCal mol - 1. The resulting reactive species consumed the ozone in different reaction pathways to give alkoxy and BrO radicals with the releasing of oxygen molecule with total enthalpy of reaction equal to - 157.9 kCal mol - 1.

دراسات حركية ثرموديناميكية لانزيم الكلوتاثيون الناقل المنقى جزئيا من مصل دم الانسان مع تاثير بعض ادوية علاج السكري

Author name: غفران عبد عمران عبد الرضا محمد الخفاجي
Supervisor name: عودة مزعل ياسر الزاملي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: This study involved (30) Person healthy (15males & 15 femals) the ages were between (20 - 25) years were obtained on samples of students from the university of Babylon / College of Science in Babel province, Iraq has been selected as control group without chronic disease and without smoking.This study attempt isolate GST enzyme from serum human .The partial purification of glutathione - S - Transferase were done using DEAE - Cellulose ,Then purification steps include precipitation by ammonium sulfate 70%, The specific activity was 0.244 U/mg protein and purification degree 1.07 folds and stepwise of Di ethyl amino ethyl - cellulose chromatography and further purified with DEAE - Cellulose column chromatography. The enzyme was apply on DEAE - Cellulose (1.5×30cm) and flow rate 1ml/min and The specific activity was 0.314 U/mg protein with recovery 55.14% and purification degree 1.50 folds.then the glutathione - S - transferase enzyme purified also from serum human by using pre - packed column affinity chromatography by containing glutathione Sepharose 4% and compare specific activity between two separation ways the activity of GST enzyme result from affinity column were more by using ion exchange column and measured of enzyme activity at 340nm by using CDNB as substrate of GST enzyme .The electrophoresis of the partial from human serum from ion - exchange chromatography and affinity chromatography in polyacrylamide gel was found that it was one protein band by using SDS - PAGE analysis by usingenzyme GST result from ion - exchange chromatography 27.7KD and affinity chromatography found (28KD). This study involved also some kinetic studies of GST , maximum activity for GST enzyme was obtained using 22.463mmol/L of 1 - chloro - 2,4 - dinitrobenzene (CDNB)as substrate ,the enzyme showed maximum activityat 35 and optimum pH at 6.8 and time at 12 minutes in incubation at 35 . Using Lineweaver - Burk plot the maximum velocity (Vmax ) and Michaelis constant Km were (11.12mmol/liter) and Vmax (1.254μmol/min) respectively .The thermodynamic constants of activation , were determined by using Arrhenius plot and found to be (35.906kJ. mol - 1, 31.73kJ.mol - 1, - 1.729 kJ.mol - 1.k ,551.40 kJ.mol - 1.k) respectively .Metformin and Dionial inhibition on the GST activity were found that , this lead to drugs effect on enzyme GST.Where showed result that non comparative inhibitor at metformin and showed that comparative inhibitor at dionial .

الاستخلاص بنقطة الغيمة لتقدير الكلور امفينيكول طيفيا في المستحضرات الصيدلانية == CLOUD POINT EXTRACTION FOR THE SPECTROPHOTOMETRIC DETERMINATION OF CHLORAMPHENICOL IN PHARMACEUTICAL PREPARATIONS

Author name: ضياء يحيى عزيز الحميدي
Supervisor name: عباس نور محمد الشريفي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: In this thesis chloramphenicol drug was determined by three methods with spectrophotometric technique.In the first method chloramphenicol was reacted with p - N,NDimethyl - aminobenzaldehyde and form yellow Schiff base product which gave higher absorbance at 436.5 nm. Schiff base reaction occurs between two compounds, one contains amino group and the other contains carbonyl group but chloramphenicol is nitro compound therefore it must convert nitro group in drug to amino group therefore reduction process to nitro group necessary for convert it to amino group.Therefore optimum conditions of reduction process were studied to know exactly the volume of concentrated hydrochloric acid which will give higher absorbance of product. Also amount of zinc, temperature of heating and time from heating during the reduction process were studied. Other optimum conditions of reaction also were studied and Calibration curve constructed and regression equation known (y = 0.0556x + 0.0246), also range of concentration which obeys Beer - Lambert Law was (0.1 - 12)ppm, Molar absorptivity (1.8 * 104 ), Sandell's sensitivity (1.8 * 10 - 2), LOD and LOQ (0.037) and (0.124) respectively. also other studies were performed such as accuracy and precision, Molar ratio method, continues variation method, reaction mechanism, Stability constant of product, Analytical applications and t - test and F - test. The proposed method was successfully in determination of chloramphenicol (CAP) in pharmaceutical preparations with good values of recovery presents (97.6% - 102.5%) and Relative Error E% between ( - 2.351 - 2.562).In the second method, chloramphenicol was reacted with 1,2 - Naphthoquinone - 4 - Sulphonic Acid Sodium Salt in basic medium by condensation reaction and form orange - red product which gave higher absorbance at 489 nm.Optimum conditions of reaction were studied and Calibration curve constructed and regression equation known (y = 0.0577x - 0.0006), also range of concentration which obeys Beer - Lambert Law was (1 - 9)ppm, Molar absorptivity (1.86 * 104), Sandell's sensitive (1.73* 10 - 2), LOD and LOQ (0.068) and (0.207) respectively. Also other studies were performed such accuracy and precision, Molar ratio method ,continues variation method, reaction mechanism, stability constant of product, analytical applications and t - test and F - test. The proposed method was successfully in determination CAP in pharmaceutical preparations with good values of recovery presents (96.149% - 103.307%) and Relative Error E% between ( - 3.851 - 3.307) In the third method, cloud point extraction was applied by extractingthe product used in the second method because there is interaction between the alkaline medium and reagent, this the interaction leads to develop colored reagent and some of radiation absorbed at maximum wavelength of product therefore used cloud point extraction to remove the interference and enhancing sensitivity of method and increasing stability of product.Chloramphenicol was reacted with 1,2 - Naphthoquinone - 4 - Sulphonic Acid Sodium Salt in basic medium by condensation reaction forming orange - red product by using same optimum condition of reaction in the second method then the product was extracted from the solution by using cloud point extraction technique.Optimum conditions of cloud point extraction were studied and Calibration curve was constructed and regression equation known (y = 0.2318x + 0.0639), the range of concentration that obeys Beer - Lambert Law was (0.1 - 6) ppm, Molar absorptivity (7.49 * 104), Sandell's sensitivity (4.31* 10 - 3), LOD and LOQ (0.032) ppm and (0.097)ppm respectively. Also Recovery of solute ( was(99.92), preconcentration factor (fc) (3.33333) and phase volume ratio (Rv) (0.3), also other studies were performed such accuracy and precision, analytical applications and test and F - test. The proposed method was successful in determine chloramphenicol (CAP) in pharmaceutical preparations with good values of recovery percent (96.091% - 101.834%) and Relative Error E% between ( - 3.909 - 1.834).Finally, this thesis presented a proposal for a new way to deal with the data in the analytical methods, which includes the new equations to find a slop and y - intercept of a straight line equation as well as introduced new parameters to determine the best linear correlation between the results, it is average of recovery (Arec), the sum of the absolute values of the relative error (SARE) in concentration computed as well as the average of the absolute values of relative error ( AARE) that gives the best results and more accurate than the usual equation.

البلمرة التكاثفية للبنتااريثريتول مع حامض الفثاليك اللامائي وتحويرة ودراسة خواصة == Condensation Polymerization of Pentaerythritol with Phthalic Anhydride and Modification and Study of its Properties

Author name: رواء حفظي زعولي
Supervisor name: محمد ناظم بهجت | ناظر نجم عبد الله
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Babylon
First pages:
Abstract: تضمن البحث تحضير الكوبوليمر المحور بخطوتين : الخطوة الاولى ، تتضمن تحضير بوليمرتكاثفي باستخدام بنتا اريتريتول وانهيدرايد الفثالك وانهيدريد الماليئك بواسطة عملية الاسترة .ان الهيكل التركيبي للبوليمر المشترك المحور الذي حصلنا عليه ، كما يلي : وشخص البوليمر المحضر بواسطة مطيافية FTIR وHNMR الخطوة الثانية ، تتضمن تحضير راتنج ذو قوام شرابي باضافة (1مول،1.5مول ،2 مول) مونومير حامض الاكريلك على التوالي الى البوليمر ، لنحصل على تلاثة انواع من الراتنج .تضمن العمل عدد من الفحوصات مثل ، الانتفاخية في الماء والتولوين والايثانول في درجات حرارية مختلفة ، الانتفاخية في محلولي بفر ذوPH مختلف وخواص قوة الشد. تم حساب معاملات الانتفاخية في الماء والتولوين والايثانول،حيث وجد ان محتوى الماء في الهلام المائي يزداد بزيادة زمن الانتفاخية . كذلك تم دراسة تا ثير درجة الحرارة على الانتفاخية في الماء والتولوين والايثانول عند درجات حرارية مختلفة تتراوح مابين 298 - 318 كلفن . تزداد معاملات الانتفاخية بزيادة درجة الحرارة وكذلك فان الكسر الحجمي للراتنج (2 Ф) تقل بزيادة درجة الحرارة .من خلال اختبارات الشد ، لوحظ ان البوليمر المحضرذو سلوك ميكانيكي لين - ضعيف للراتنج المحتوي على الاكريلك اسد. | In this work, a new modified Co - polymer was prepared by condensation polymerization by using phthalic anhydride, pentaerythritol and maleic anhydride through esterification reaction.The structure of modified co - polymer was : Identification of modified polyester resin by FT - IR, 1H - NMRA preparation of pourable syrup resins by the addition of (1, 1.5 and 2 moles) acrylic acid monomer respectively, to the modified polymer, to give three types of resins.Many tests were carried out, i.e., swelling degree in water, toluene and ethanol at different temperatures, and swelling at two different PH. Also the tensile properties of the prepared polymers have been studded.The swelling parameters in water, ethanol and toluene were calculated. The water content, of hydrogels increased with increasing time of swelling. The effect of temperature on the swelling in water, ethanol and toluene at different temperatures ranging from 298 to 318 K was also studied. The water, ethanol and toluene content have been increased with increasing temperature. While the volume fraction of the resins (Ф2) have been decreased with increasing temperatures. From the tensile tests, it was found that the prepared polymer; have soft - weak behavior.

تحضير وتشخيص وتقيم الفعالية البيولوجية لبعض مركبات الفورمازان المشتقة من قواعد شف الجديدة ومعقداتها مع بعض العناصر الانتقالية == Synthesis, characterization and biological evaluation of some new Formazan compounds derived from Schiff Bases and their complexes with some transition Metals.

Author name: اعراف محمود داود
Supervisor name: حيدر عباس مهدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Dhi Qar
First pages:
Abstract: This thesis contains three chapters represents, the first chapter introduction and interested in studying the chemistry of schiff base and derivatives of formazan, their complexes in terms of their characteristics, importance and synthesis.The second chapter is interested in describing the chemicals and procedures used in the synthesis of the required compounds, and the study of physical measurements, synthesis methods of compounds and evaluation as well as the biological activity.In this research, four new derivatives of formazan (L3, L4, L5 - 4d), which synthesized from the reaction of Diazonium salt amine with suitable Schiff base (L1, L2 - 2d). The Schiff base can product of different primary amines with several aromatic aldehyde and synthesized both of the (Schiff bases, formazans) suitable complexes.The third chapter Results and Discussion, identified synthesized formazan derivatives as well as Schiff bases prefix and its complexes by appropriate spectral methods including of infrared spectroscopy (FT - IR) for all compounds, Nuclear Magnetic Resonance spectrum (1H - NMR) for all compounds Microanalysis (CHNS) for the majority of compounds as well as Mass spectra. For all complexes were recording certain physical properties, such as melting point (m.p.). Monitoring progress of the chemical reaction by using thin chromatography layer (TLC). We synthesis eight complexes (three from Schiff bases and five from formazan derivatives) were complexes with ions (Co, Ni, Cd), then measuring the molar conductivity of complexes. Then study the biological effectiveness for some compounds have been chosen complexes Schiff bases, as well as formazan complexes to determine the effect of active groups in these compounds to evaluate the efficiency ofXIthe compounds against different type of bacteria.The research also includes a test of biological effectiveness of the prepared ligands and their metallic complexes, where we study response inhibitory to the three types of bacteria, a gram positive type of bacteria (Staphylococcus aureuse) and gram negative type of the bacteria (Escherichia Coli and salmonella species) and compared with the standard inhibitor (Cipro).The biological effectiveness swohs positive results as it was noted The ligand L1, L2, L3, L4, L5 and Schiff base 4d Showed lower efficiency than the standard inhibitor trend three types of bacteria. The prepared complexes from ligands appeared high effective than the effectiveness of the ligands itself The formazan (L3, L4, L5 dna 2d) appeared high effective than the effectiveness of the prepared Schiff base

دراسة كيمو حيوية مقارنه للاجهاد التاكسدي وانماط الدهون في المرضى كبار السن المصابين بمرض الارتجاف الاذني في محافظة ذي قار العراق == A Biochemical Comparative Study of Oxidative Stress and Lipid Profile in Elderly Patients With Atrial Fibrillation in Thi - Qar Governorate/Iraq

Author name: سارة عاشور ساير
Supervisor name: رائد معلك حنون الصالح | عدنان الطعان الخفاجي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Dhi Qar
First pages:
Abstract: Atrial fibrillation (AF) is the most common cardiac arrhythmia in the general population, and a major cause of morbidity and mortality. Lifetime risk for development of AF has been estimated to 1 in 4 in individuals aged 40 years or more.The present study is designed to determine the levels of oxidative stress by measuring lipid peroxidation product (malondialdehyde MDA), antioxidant state by measuring some antioxidants such as (ceruloplasmin Cp, Transferrin Tf, albumin Alb ,uric acid Ua) ,in addition to lipid profile (cholesterol TC, triglyceride TG, high density lipoprotein cholesterol HDL - C, low density lipoprotein cholesterol LDL - C and very low density lipoprotein cholesterol VLDL - C) in atrial fibrillation patients .The study included (150) subjects; (75) normal subjects (control) and (75) patients with atrial fibrillation. The patients are divided into two groups according to the age : (39) elderly patients [the age range (60 - 80) years] and (36) others patients [the age range (20 - 59) years], also patients are divided in to two groups according to the age with one or more risk factor (Hypertention (HTN), Ischemic Heart Disease(IHD), Heart Hailure (HF)) : elderly which included (18) patients (lone AF) , (21) patients (AF with HTN, IHD, HF) and others which included (17) patients (lone AF), (19) patients (AF with HTN, IHD, HF).The normal subjects (control) also divided into two groups according to the age : elderly [the age range (60 - 80) years] and others [the age range (20 - 59) years] .According to age, the results shown significant increase in the concentration of serum (MDA, Cp, uric acid, TC, TG, VLDL - C, LDL - C ) in elderly and other groups in comparison with their control groups (p≤0.05). It was found significant increase in the concentration of serum MDA in elderly group in comparison with other group, also it was found significant increase in the concentration of serum uric acid in control elderly group in comparison withXIVcontrol other group (p≤0.05). The results also showed non significant differences in the concentration of serum (Cp, uric acid, TC,TG, LDL - C, VLDL - C) between elderly and other groups. It was also found non significant differences in the concentration of serum ( Cp, TC, TG, LDL - C, VLDL - C) between control elderly and control other groups (p≤0.05). While serum Alb , serum Tf and serum HDL - C concentrations show a significant decrease in elderly and other groups in comparison with their control groups (p≤0.05). The results showed significant decrease in the concentration of serum HDL - C in control elderly group in comparison with control other group. Also there were no significant differences in the concentration of serum Alb serum Tf and serum HDL - C between elderly and others groups (p≤0.05).According to the age with one or more risk factor (HTN, IHD, HF) the results show a significant increase in the concentration of serum (MDA, Cp , uric acid, TC, TG, VLDL - C , LDL - C ) in elderly and other groups in comparison with their control groups (p≤0.05). It was found a significant increase in the concentration of serum MDA in the groups AF and AF with HTN, IHD, HF ( in elderly groups) in comparison with groups AF and AF with HTN, IHD, HF (in other groups) respectively (p≤0.05). It was also found a significant increase in the concentration of serum uric acid in control elderly groups in comparison with control other groups , also there were no significant differences in the concentration of serum (CP ,TC , TG ,VLDL - C, LDL - C) between elderly and other groups (p≤0.05). serum Alb ,serum Tf and serum HDL - C show a significant decrease in elderly and other groups in comparison with their control groups, also there was significant decrease in the concentration of serum HDL - C in control elderly groups in comparison with control other groups (p≤0.05). It was also found non significant differences in the concentration of serum Alb and serum Tf between elderly and other groups (p≤0.05).

تخليق قواعد شف جديدة مشتقة من انهدريد البايرومليتك == Synthesis ,Antibacterial of Some Novel Schiff Bases Derived From Pyromellitic Dianhydride

Author name: عذراء محمد سلوم
Supervisor name: امينة عبد الرحمن فياض | عماد تقي علي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Baghdad
Language: English
University location: Baghdad
First pages:
Abstract: تم تخليق قواعد جديده مشتقة من انهدريد ثنائي البايرومليتك بعدة خطوات. حيث حضرت مشتقات حامض البايرومليتك المتناظره a­c[ I ] من تفاعل انهدريد ثنائي البايرومليتك مع بعض الامينا ت الاورماتية الحاويه على (مجاميع ساحبه واخرى دافعة ) في الاسيتون كمذيب. واشتملت | The novel Schiff bases derived from pyromellitic dianhydride were synthesized by several steps reaction. A symmetrical diamic acide [I ]a - c was synthesized by the reaction of pyromellitic dianhydride with some aromatic amines (containing electron withdrawing , repulling groups ) in dry acetone.In the second step the diacids were converted to their corresponding diimide [II ]a - c using acetic anhydride and sodium acetate system as a dehydrating agent, via the intramolecular cyclization steps of amic acids.The third step was to synthesis the hydrazone derivatives from the reaction of diimides , with 80 % hydrazine hydrate at (50 - 60)C?.These hydrazone derivatives were allowed to react with several aromatic aldehydes to form new Schiff bases via step four at a temperature near by (80 - 85)C?. As shown in the following scheme (3.1). All the novel compounds and their structures have been ascertained by their melting points , mixed melting points , C.H. N analysis , FTIR , UV - Viss. and 1HNMR spectroscopy for some of them. Also the biological activity of some of them was studied which showed that these compounds have different activities towards the studied bacteria.

دراسة تاثير الفسفاتين وبعض المتغيرات الحياتية على مرضى سوفان المفاصل المصابين وغير المصابين بداء السكري من النوع الثاني == A Study of Visfatin And Some Biochemical Variables In Osteoarthritis With And Without Diabetes Mellitus Type2

Author name: لمياء شاكر عاشور
Supervisor name: طارق محمد علي رجب الحكيم | حامد غفوري حسن
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
University: University of Baghdad
Language: English
University location: Baghdad
First pages:
Abstract: يتضمن هذا الفصل مقدمة عن المركبات الدوائية الاتية وطرائق تقديرها وهي : • الترايفلوبيرازين هيدروكلوريد Trifluoperazine Hydrochloride • طرائق تقدير للترايفلوبيرازين هيدروكلوريد Methods for the determination of Trifluoperazine hydrochloride • الكلوربروم | This thesis consists of four chapters : Chapter one : contains introduction about drug compounds listed below - Trifluoperazine hydrochloride. - Methods for the determination of Trifluoperazine hydrochloride. - Chlorpromazine hydrochloride. - Methods for the determination of Chlorpromazine. - Aim of the research.Chapter two The Chapter includes the development of a new sensitive spectrophotometric method for the determination of a Trifluoperazine hydrochloride in aqueous solution. The method is based on the oxidative coupling reaction of Trifluoperazine hydrochloride with Sulphanilic acid reagent in a acidic medium pH 1.4 in the presence of Potassium Iodate to produce an intense violet coloured, water soluble and stable product , which exhibits maximum absorption at 544 nm. Beer’s law is obeyed over the arange 12 to 66 µg.ml - 1 of Trifluoperazine hydrochloride, with a molar absorptivity of 4804 L.mo1 - 1.cm - 1 , Sandell’s sensitivity index of 0.01 µg.cm - 2 , relative error range not more than 1.26% , and D.L 0.495 µg.ml - 1. The method has been successfully applied for the determination of Trifluoperazine hydrochloride in tablets.Chapter threeThe Chapter includes the development of a sensitive spectrophotometric method for the determination of Trifluoperazine hydrochloride in aqueous solution based on reduction of Fe3+ with Trifluoperazine hydrochloride. The Fe2+ formed is complexed with 2,2’ - bipyridyl at pH 4.2 to produce a red , water soluble and stable complex, which exhibits maximum absorption at 524 nm. Beer’s law obeyed in the concentration range from 2 to 50 µg.ml - 1 of Trifluoperazine hydrochloride. The molar absorptivity is 5284.4 L.mol - 1.cm - 1 and Sandell’s sensitivity index of 0.090 µg. cm - 2 , relative error from 1.64 % , and D.L 0.788 µg.ml - 1. The method has been successfully applied to the determination of Trifluoperazine hydrochloride in tablets.Chapter FourThe Chapter includes the development of a new sensitive spectrophotometric method for the determination of a Chlorpromazine hydrochloride in aqueous solution. The method is based on the oxidative coupling reaction of Chlorpromazine hydrochloride with Sulphanilamide reagent in a acidic medium pH 3.2 in the presence of Ammonium ceric Sulphate dihydrate to produce an intense violet coloured, water soluble and stable dye, which exhibits maximum absorption at 530 nm. Beer’s law is obeyed over the arange 6 to 66 µg.ml - 1 of Chlorpromazine hydrochloride, with a molar absorptivity of 2842.28 L.mo1 - 1.cm - 1 , Sandell’s sensitivity index of 0.1250 µg.cm - 2 , relative error range not more than 2.49 % , and D.L 1.2028 µg.ml - 1. The method has been successfully applied for the determination of Chlorpromazine hydrochloride in tablets.

تحضير دقائق مغناطيسيه متناهيه الصغر (نانو) ودراسة تقييدها لانزيم الزانثين اوكسيديز == Prepared of Magnetic Nanoparticles And Study The Immobilized For Xanthine Oxidase

Author name: مصطفى محمد كريم
Supervisor name: حسين كاظم الحكيم
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Najaf
First pages:
Abstract: The purpose of this thesis is to report quantum chemical investigations into a series of problems related to contemporary organometallic chemistry. In recent years density functional approaches have become the most commonly used theoretical methodology in organometallic chemistry. Alongside these developments, a number of new tools for analyzing electronic structure such as topological analysis of electron density (Atoms in Molecules theory) have emerged. As a result, theory is now in a position to compute ab initio many of the experimental observables that underpin modern organometallic chemistry.The bonding in the Triosmium carbonyl cluster 1 [Os3(? - H)(? - ?2 - dpa - N,N)(CO)10] and Triosmium carbonyl cluster 2 [Os3( ? - H)2(NHC)(CO)9] are explored using the Quantum Theory of Atoms - in - Molecules (QTAIM). The metal - metal and metal - ligand bond critical points properties ?(r), ?2?(r), H(r), G(r), V(r) and ellipticity, and also the bond delocalization indices ?(A, B), are correlated with the data from previous studies of the organometallic systems. These results have allowed a comparison between topological properties of different atom - atom interactions. In the core of dihydride triosmium cluster 2, Os3H2 part, the topological data recognizes the existence of a bond path in the dihydride bridged Os atoms, Os(1) - Os(3) edges, whereas in monohydride triosmium cluster 1 there is no direct bond path has been found for the interaction between the hydride bridged Os atoms, although a non - negligible delocalization index ?(Os(1)...Os(2)) has been obtained for this non - bonding interaction. A multicenter 4c - 4e interaction is proposed to exist in the core part, Os3H, in cluster 1 and bridged part, Os(1) - H(1) - Os(3) - (H2) in cluster 2. In addition, an interaction of 5c - 5e type is proposed to exist in the core part, Os3H2. All topological parameters calculated for the Os - N and Os - C bonds between the osmium atoms and the pyridyl and NHC ligands in compound 1 and 2, respectively, are similar, and they confirm that these interactions are pure ? bond. The analysis of the topological parameters of the NHC and pyridyl ligands bonds confirm the existence of ? - electron delocalization within the six - membered ring of pyridyl ligand and hindered ? - electron delocalization within the five - membered ring of NHC ligand with some double - bond character in the interaction of the carbine C atom with the adjacent N atoms.

دراسة حركية لتاثير بعض المركبات المخفضة للدهون الثيازينات والثياديازول على الكرياتين كاينيز و3 - هيدروكسي - 3 - مثيل كلوتاريل كو انزيم - اي ريدكتيز في امصال مرضى ارتفاع الدهون والفئران المختبرية التي تم حث ارتفاع الدهون فيها == Kinetic Study of The Effect of Some Novel Lipid Lowering Thiazines And Thiadiazole Compounds On Creatine Kinase And 3 - Hydroxy - 3 - Methyl - Glutaryl - Coa Reductase Activities In Sera of Hyperlipidemia Patient’s And Wister Mice With Induced Hyperlipide

Author name: تمارة احمد عبد الكريم العبيدي
Supervisor name: زينب منيب مالك الربيعي | غيد حسان عبد الهادي العبيدي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: تمثل الستيرويدات فئة هامة من العقاقير الطبيعية وكذلك الصناعية نظرا لقدرتها على اختراق الخلايا واداء بعض الوظائف البيولوجية الاساسية وبشكل رئيسي هي عوامل مضادة للفيروسات ومضادات للاورام. وتقسم الرسالة الحالية على ثلاثة فصول.يمثل الفصل الاول مقدمة عامة حو | Steroids represent an important class of natural as well as synthetic drugs because of their ability to penetrate cells and perform some of the most fundamental biological functions mainly as antitumor and antiviral agents. The present thesis is devided into three chapters.The first chapter represented a general introduction concerning the structures of some potent steroids, and the pathways of the synthetic adrenal steroids as well as their pharmacological importance in medicine, in general. This part is focused mainly also on the pregnenolone as an important potentially active steroid, including its structural modification at the hydroxyl and keto groups at C - 3 and C - 20 and their uses as antitumor agents. Mitsunobu, Suzuki reactions and aldol condensation as well as chalcon formation and their application at steroids have been described. The second chapter is concerned with the experimental work which included different synthetic methodology.The third chapter is the main part of the thesis, described the synthesis of new 3? - pregnenolone ester derivatives at C - 3 via Misunobu reaction of the carboxylic acid derivatives, such as : rhodamin B, indomethacin, naproxen, protocatecuic acid, vanillic acid and p - coumaric acid, which showed inversion in configuration at the ester group at C - 3. In addition, the synthesis of 17 - (4 - chloro - chalconyl)pregnen - 3? - ol has been described, which then treated with various substituted phenylboronic acids such as : 2,4 - difluoro - , 5 - carboxy - 3 - nitrop - ,4 - fluoro, 4 - thiomethyl - , 4 - hydroxy - , 2,4, - dimethoxy - , 4 - trimethylsilyl, 2 - triflouromethyl - , 3 - cyano, 4 - ethoxyphenyl boronic acids under Suzuki cross - coupling reaction conditions using Pd(PPh3)4 as a catalyst and Na2CO3 as a base to give the (E) - 3 - (substituted - [1,1’ - biphenyl] - 4 - yl) - 1 - (3? - hydroxy - pregnen - 17 - yl) - prop - 2 - en - 1 - one. Two compounds, 17 - acetyl - 5 - pregnen - 3? - yl) - 2 - (2,6 - bis(diethylamino) - 9H - xanthen - 9 - yl)benzoate, and 17 - ((E) - 3 - (4 - chlorophenyl)acryloyl) - 5 - pregnen - 3? - yl) - 2 - (2,6 - bis(diethylamino) - 9H - xanthen - 9 - yl)benzoate have been synthesized via coupling reaction using DCC as a coupling reagent to afford these ester with retention in configuration, aiming to study their fluorescence properties. Moreover, tritylation of the pregnenolone has been described to protect the alcohol at C - 3 during the structural modification of keto group at C - 20 under basic medium. The structures of all the synthesized compounds have been assigned from their 1H, 13C, and 2D NMR (HSQC, HMBC, COSY, NOESY) spectroscopy as well the as theoretical calculations of the HOMO and LUMO energies of the trans and cis isomers of the chalconyl pregnenolone aryl derivatives to compare them with the NMR data, which showed that trans isomer is energetically more favoured.Furthermore, the flourescence proroperties of the two rhodainyl pregnenolone esters have been studies which one show remarkable quantum yield (?F) in comparison to Rhodamin B itself.The anti - HIV activity of some arylated chalconyl pregnenolone derivatives have been studies and one of these analogues having diflouro substituents exhibited remarkable activity against HIV - 1 and 2. Therefore, the molecular modeling study of this analogue is performed and showed two hydrophobic interactions and one hydrogen bonding with the amino acids residues of the reverse transcriptase enzyme of HIV.

تحسين حماية التاكل للمعادن (الخارصين، النحاس، الالمنيوم، الحديد الكربوني والحديد المقاوم للصدا 316) في ماء البحر الصناعي باستخدام الطلاء بالمواد النانوية == Corrosion Protection Enhancement Of; Zn, Cu, Al, Carbon Steel And Stainless Steel 316 In Artificial Seawater By Coating With Nanomaterials

Author name: رائد عبد شاكر محمود
Supervisor name: عبد الكريم محمد علي جبر السامرائي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: الهدف من هده الدراسة هو تقدير تاثير بعض مشتقات الثياديازول والثيازين الجديدة التحضير على فعالية كل من الانزيمين الكرياتين كاينيز و3 - هيدروكسي - 3 - مثيل كلوتاريل كو - انزيم اي ريدكتيز بالاضافة الى قياس صورة الدهون في مرضى ارتفاع الدهون والفئران المختبرية | The aim of this study is to evaluate the effect of some novel prepared derivatives of thiadiazole and thiazine on the activities of creatine kinase (CK) and 3 - hydroxy - 3 - methylglutaryl CoA reductase(HMGR) in addition to lipid profile in sera of hyperlipidemic patients and in mice induced hyperlipidemia by feeding cholesterol rich diet.The study includes two parts; in vitro study : Sixty individuals with age ranged between (40 - 60) years were enrolled in this study. They were divided into two groups; first group (G1) consists of 30 healthy individuals as a control group with body mass index (BMI) (25.67). The second group (G2)consists of 30 patients with hyperlipidemia and BMI (26.48) which diagnosed by physician. The patients attended the Ibn - Al Naphes hospital during November 2013 to February 2014. Patients with high blood viscosity, diabetes mellitus, renal failure as well as those who are under treatment with statins were excluded. The serum which obtained used in the determination of lipid profile[total cholesterol(Tch),triglyceride(TG), high density lipoprotein(HDL - c), very low density lipoprotein(VLDL - c)], fasting blood glucose(FBG), aspartate transaminase (AST), alanine transaminase(ALT) and C - reactive protein(CRP).Four organic compounds 3 - (4 - (dimethylamino) phenyl) - 2,3 - dihydro - 2 - (3 - nitrophenyl benzo[1,3 - e]thiazin - 4 - one[I], 5 - (4 - imethylamino)benzylideneamino) - 1,3,4 - thiadiazole - 2 - thiol[II], 2 - (4 - dimethylamino)phenyl) - 2,3 - dihydro - 3 - (5 - mercapto - 1,3,4 - thiadiazol - 2 - yl)benzo[1,3 - e]thiazin - 4 - one[III], and N - (4 - (dimethyl amino)benzylidene) - 5 - (isopropylthio) - 1,3,4 - thiadiazole - 2 - amine[IV] were used in this study to test their antihyperlipidaemic ability and their effect on CK and HMGR activities. The results revealed that compounds(III and IV)showed an activation effect in all concentrations on CK and HMGR activities, while compounds(I and II) showed an inhibitory effect in some concentrations for CK and in all concentrations for HMGR. Therefore, compounds (III and IV) were excluded from this study. The results showed that (10 - 4M) for compound I and (10 - 5M) for compounds II give the best inhibition percentage among the other concentrations on CK and HMGR activities which the kinetic study throughout with these concentrations for these compounds. Simvastatin, which considered as standard drug for lipid lowering, was used for comparsion with the potency of compounds I and II on HMGR activity in treatment of hyperlipidaemia. The results showed an inhibitory effect of simvastatin on HMGR activity with percentage inhibition 88%. The effect of compounds (I and II) on ALT and AST were examined in (10 - 4 M) for compound I and (10 - 5M) for compound II in vitro study. The results showed the inhibitory effect of compounds I in concentration (10 - 4 M) and compound II in concentration (10 - 5M) on ALT and AST activities.The Vmax, Km and type of inhibition for compounds I and II on CK and HMGR activities were studied by using Lineweaver - Burk plot. The results showed that also compound I at 10 - 4M was considered to be a noncompetitive inhibitor for CK activity with Vmax values (1000 and 344.82)U/L for uninhibited and inhibited enzyme respectively and Km value (10) mmol/L. The results also showed that compound II at concentration 10 - 5M was considered to be a competitive inhibitor for CK activity with Vmax value (588.23)U/L and Km values (5.51 and 4)mmol/L for the uninhibited and inhibited enzyme respectively.In vitro, the effect of compound (I) with concentration (10 - 4M) and compound (II) with concentration (10 - 5M) were examined in vivo study. The study was carried out with sixty male Wister mice aged seven to eight weeks and theirweight were (180 - 200 g) ,obtained from animal house , in College of Medicine, Baghdad University. The mice were grouped as follow : group one (12 mice) as control group, group(2) : consists of 48 mice in which the mice were daily administered cholesterol (25mg/k/day), in coconut oil 6% and creamy cheese for 28 days. Lipid profile were measured for twelve mice chosen randomly from G2 to diagnosis hyperlipidemia. Then group2 is subdivided into three groups as follows : group (2.A) : (12 mice) as positive control group in which the mice were daily administered simvastatin (40mg /day) as standard drug for hyperlipidemia, group 2B : (12 mice) in which the mice were daily treated with (10 - 4)M of compound (I)via drinking water for 20 days and Group(2.C) : (12 mice) in which the mice were daily treated with (10 - 5)M of compound II for 20 days. The results showed significant elevation in levels of Tch, TG, LDL - c and VLDL - c, while there is significant reduction in HDL - c levels in G2 comparing to control group(G1), after administration of fat rich diet. Simvastatin, compound I with concentration (10 - 4M) and compound II with concentration (10 - 5M) were administrated to G2A, G2B and G2C respectively. Also, the results showed that the activities of CK reduced for group G2B and G2C while it is increased for G2A. The results also showed that the activities of HMGR were reduced in the three treated groups. The results revealed that compounds I and II exhibit more potent antihyperlipidaemic effect than simvastatin. Also, compound I showed more potent antihyperlipidaemic effect than compound II.The results revealed that compounds I and II showed a noncompetitive inhibitor effect on CK with Vmax values(1000and 166.6) U/L for uninhibited and inhibited enzyme respectively and Km value (0.6) mmol/L for compound I, and with Vmax vales (1000 and 250)U/L for uninhibited and inhibited enzyme respectively and Km value (0.84) mmol/L for compound II.In conclusion, the novel synthetic compounds (I and II) seem to be of interest in the development of new antihyperlipidaemic agents that exhibit inhibition effect on CK while statins cause increase in this enzyme. Also these compounds exhibit inhibition effect on HMGR activity more than simvastatin, which is a key enzyme in cholesterol synthesis.

تحضير ,تشخيص, دراسة فعالية مضادة للاكسدة ومضادة للسرطان لمعقدات الذهب (III) مع مركبات حلقية غير متجانسة == Synthesis ,Characterization ,Antioxidant And Anti - Cancer Activity Studies of Gold (III) Complexes With Heterocyclic Compounds

Author name: اية جمال عبد الحميد
Supervisor name: فراس عبد الله حسن
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
Language: English
University location: Baghdad
First pages:
Abstract: تضمن موضوع البحث تحضير مركبات حلقيه خماسية وسباعية غير متجانسة متنوعة،من خلال اربعة اجزاء هي : الجزء الاول : - تضمن هذا الجزء تحضير مركبات مشتقات 1, 3, 4 - اوكسادايزول من مركب (ثنائي اثيل مالونيت)، كما موضح بالمخطط (1).الجزء الثاني : - تضمن هذا الجزء تحض | This work involves synthesis of different five, and seven membered heterocyclic rings, and divided into four different parts and the reaction steps for each part are summarized as shown below.First part : This part involved the synthesis of 1,3,4 - Oxadiazoles derived from diethyl malonate.Scheme (1).Second part : This part involved the synthesis of Oxazepine , tetrazoles, and thiazolidinone,from 4,4' - ((((methylenebis(1,3,4 - oxadiazole - 5,2 - diyl))bis(3,1 - phenylene))bis(azanylylidene))bis(methanylylidene))bis(N,N - dimethylaniline).(Scheme 2).Third part : This part involved the synthesis of 1,1' - (1,4 - phenylene)bis(N - substitutedmethanimine) [C1 - 9] from terephthalaldehyde. (Scheme 3). Fourth part : This part involved the synthesis of 1,3,4 - Oxadiazoles derived from terephthalaldehyde and hydrazone carboxamide.In addition, this part deals with the evaluation of antibacterial activities of some of the synthesized compounds. These activities were determined in vitro using disc diffusion method against four pathogenic strains of bacteria (E.coli a, Pseudomonas, Bacillus, and Staphylococcus.), the results revealed that some of these compounds showed measurable activity. (Scheme 4).The liquid crystalline behaviors of the two series have been examined by means of hot - stage polarizing microscopy for the determination of phase transition temperatures and the type of mesophases. The prepared compounds are characterized through determining their melting points, colors physical properties) and (FT - IR, 1H - NMR,) spectroscopy, (C.H.N.S, DSC) analysis and checked by T.L.C.

دراسة البلمرة الكهروكيمياوية وخواص حماية التاكل لطلاء متعدد البايرول على الفولاذ الكاربوني والفولاذ المقاوم للصدا == An Investigation of Electropolymerization And Corrosion Protection Properties of Polypyrrole Coating On Carbon Steel And Stainless Steel

Author name: رواء عباس محمد
Supervisor name: عبد الكريم محمد علي جبر السامرائي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: تم تحضير سلسلة من مشتقات 1, 2, 4 - ترايزول بواسطة تفاعلات الغلق ,حضر حامض البنزويك هيدرازايد (1) بواسطة تفاعل مثيل بنزويت مع الهيدرازين ثم تفاعل المركب (1) مع CS2 في محلول كحولي قاعدي ليعطي ملح البوتاسيوم (2). حضر المركب (3) بواسطة غلق ملح البوتاسيوم (2)م | A series of 1,2,4 - triazole derivatives were synthesized by cyclization reaction, the benzoic acid hydrazide (1) was synthesized by reaction of methyl benzoate with hydrazine hydrate then compound (1) was reacted with CS2 in solution of alkali ethanol to give potassium dithiocarbazinate salt (2) , the basic nucleus 4 - amino - 5 - phenyl - 1 - 4H - 1,2,4 - triazole - 3 - thiol (3) was prepared by cyclization of potassium salt (2) with hydrazine hydrate using water as solvent under reflux condition. compound (3) was subjected to addition reaction with different aromatic aldehydes to synthesize Schiff bases (4a,b) which were cyclized by treating with thioglycolic acid to prepare compounds (5a,b).compounds (6) and (7) obtained by cyclization reaction of compound (3) with urea and thiourea. Also in this research, 1,3,4 - thiadiazole derivatives were synthesized by cyclization of thiosemicarbazied with substituted carboxylic acid and sulphuric acid, to yield 2 - amino - 5 - R - 1,3,4 - thiadiazole (8). Schiff bases formation (9a,b) were by reflux of aromatic aldehyde with 2 - amino - 5 - R - 1,3,4 - thiadiazole (8) in the presence of absolute ethanol. Compounds (10a,b) were prepared by cyclization reaction of compounds (9a,b) with thioglycolic acid.The Synthesized compound were confirmed by their melting point ,FTIR ,U.V - visible ,1HNMR spectra and evaluated for their antioxidant activity by using stable free radical 1,1 - diphenyl - 2 - picryl - hydrazyl DPPH. of all tested compounds. compound (5b) was the most active in all concentrations compared to standard Ascorbic acid with an IC50 value 5.84 ?g/ml. In this study, the cytotoxic effects for compounds (5a),(5b),(6),(7),(10a),(10b) were studied in one cultured cellular models (MCF7 cell line) breast cancer (at different concentration) compared to doxorubicin as positive control by cell viability assay (MMT assay), compound (5b) showed the highest cytotoxicity effect with an IC50 value =56.98?g/ml.Also, we examine the cytotoxic effects of gold III complex (AuL2) of bi - dentate ligand (5a) in one cultured cellular models (MCF7 cell line) by High Content Screening and analysis (HCS). The inhibitory effect of AuL2 on breast cancer cell growth was due to induction of apoptosis as evidenced by Annexin V staining and cell shrinkage. We found that AuL2 - mediated lead to disruption of mitochondrial membrane potential (MMP), cell membrane permeability, and release of cytochrome c from the mitochondria into the cytosol. suggesting (AuL2 ) as a potential MCF7 inhibitor. Thus, we suggest that (AuL2) may have therapeutic value in breast cancer treatment worthy of further development. Bis(2 - (4 - Dimethylamino - phenyl) - 3 - (3 - mercapto - 5 - phenyl - [1,2,4]triazol - 4 - yl) - thiazolidin - 4 - one)gold(III) chloride. monohydrate

تقدير التعكرية لفصائل منتخبة باستخدام التشعيع بمصفوفة من ثنائي وصلة باعث وبمتحسسات شمسية بتقنية الحقن الجرياني المستمر : دراسة وتطبيق == Turbidimetric Determination of Some Selected Species Via The Use of Linear Array Light Emitting Diode Irradiation With Solar Cell In Continuous Flow Injection Analysis : Study And Application

Author name: محمد كاظم حمود
Supervisor name: عصام محمد علي شاكر الهاشمي
General topic: Chemistry
Specific topic: Chemistry
Degree: Master
Language: English
University location: Baghdad
First pages:
Abstract: في هذا البحث تم تقدير المركبات(SMX,TMP,CAF,HYO and PAR) باستخدام المشتقات الطيفية (الاولى , الثانية ,الثالثة والرابعة). على شكل امزجة ثنائية للادوية بواسطة تطبيق التقاطع الصفري كما يلي : 1 - مزيج السلفاميثاكسازول والترايميثوبريم باستخدام المشتقة الاولى و| This research includes determination of drugs SMX, TMP, CAF, HYO and PAR using derivative spectrophotometry (first, second, third and fourth derivative) were developed for binary mixture by applying zero - crossing technique for pure synthetic mixture and their pharmaceutical formulation as follows : 1. SMX with TMP mixture : SMX was determined by applying 1D&4D teach s at 288.0 and 257.8 nm (zero crossing point of TMP) with linear concentration ranges (2 - 30) and (2 - 25) mg/L , r = 0.9996 and r = 0.9992 LOD = 0.750 and LOD = 0.360 mg/L and TMP was determined by applying 4D teach at 251.5 nm (zero crossing point of SMX) with concentration range (2 - 30) mg/L , r = 0.9995 and LOD = 0.382mg/L. The RSD were 0.255, 0.280 and 1.136 for SMX and TMP respectively and applied for (TRIMOL - 400SMX, 80TMP mg) and (METHOPRIM - 400SMX,80TMP mg).2. PAR with CAF mixture : PAR was determined by applying 3D teach at 275.8 nm (zero crossing point of CAF).With linear concentration range (2 - 35) mg/L , r = 0.9987and LOD=0.445mg/L. And CAF was determined by applying 4D teach at 294.7 nm (zero crossing point of PAR). With linear concentration range (2 - 35) mg/L , r = 0.9995 and LOD = 0.162 mg/L. The RSD was 0.222 for PAR and 0.130 for CAF and applied for (PANADOL EXTRA - 500PAR, 65CAF mg).3. PAR with HYO mixture : PAR was determined by applying 1D&2D teach s at 297.4 and 303.5 nm (zero crossing point of HYO) with linear concentration ranges (2 - 30) and (2 - 30) mg/L , r = 0.9998 and r = 0.9987 LOD = 0.081 and LOD = 0.250 mg/L and HYO was determined by applying 1D teach at 215.9 nm (zero crossing point of PAR) with concentration range (2 - 25) mg/L , r = 0.9997 and LOD = 0.091mg/L. The RSD were 0.107, 0.400 and 0.342 for PAR and HYO respectively and applied for (SPAZMOTEK PLUS - 500PAR,10HYO mg). This thesis has mainly been structured in three different chapters, each one containing the following information : Chapter one provides a short historical review with the analytical performance characteristics of UV - visible are described. The applications of UV and DS in pharmaceutical and SMX, TMP, CAF, HYO and PAR analyses and their mixture.the general and specific objectives of thesis are reported. Chapter two corresponds to the experimental part. Reagents, instruments, procedures and detail protocols for the preparation of standard solution and pharmaceutical sample which used in this study are reported.Chapter three contains the experimental results and discussion that lead to the possibility of successful applications which used DS to determine the concentration of each material in drugs.

نمط جديد للتحليل بالحقن الجرياني المستمر باستخدام نظام تشعيع متعدد القنوات مرتبة بهيئة مصفوفة خطية واثنان من الخلايا الشمسية لقياس التعكرية لتقدير الفصائل التحليلية ذات الاهمية : دراسة وتطبيق == New Mode of Cfi Analysis Using Multiple Channel Irradiation System In A Linear Array Arrangement With Twin Solar Cells For Turbidimetric Determination of Analytically Interesting Species : Study & Application

Author name: عمر اياد ياسين القيسي
Supervisor name: نغم شاكر تركي العوادي
General topic: Chemistry
Specific topic: Chemistry
Degree: Doctorate
Language: English
University location: Baghdad
First pages:
Abstract: الفصل الاول : يشمل الفصل الاول مقدمة عن تفاعلات الترسيب، مبادئها، ميكانيكية تكوين الرواسب، انواع الرواسب. وكما يتضمن الفصل الاول مقدمة عن الضوء والنظرية الكهرومغناطسية، وتداخل الضوء مع المادة (الانعكاس، الانكسار، النفاذية، الامتصاص). ناقش الفصل الاول بشكل
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