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تحضير وتشخيص الدقائق النانوية لاوكسيد النحاسوز بواسطة الكتروليتات مختلفة == Preparation And Characterization of Cuprous Oxide Nanoparticles By Different Electrolytic Media
Author name:
حيدر خضير خطار
Supervisor name:
فؤاد عبد الامير السعدي | سامي وحيد راضي الحسناوي
General topic:
Chemistry
Specific topic:
Physical Chemistry
Degree:
Master
University:
University of Kufa - College Of Science For Girls - Chemistry Department
Language:
English
University location:
Najaf
First pages:
25T1438 - p.pdf
Abstract:
في الواقع، لم تلقي عملية فصل واستخلاص الكميات الضئيلة من الادوية في العينات الحيوية وكذلك في المستحضرات الصيدلانية اهتماما واسعا وكبيرا باستعمال مايسمى الاستخلاص بنقطة الغيمة. وفي هذا الصدد، نعتقد ان العمل البحثي الحالي سوف يسهم في فتح افاق جديدة في تصم | The separation and extraction of trace amounts of medicaments in biological specimens, as well as in pharmaceutical formulations have not received much attention by using the so - called cloud - point extraction (CPE). In this context, we think that the present research work will contribute to opening new prospects in designing procedural steps and expands the applications of the cloud point extraction methodology in most important areas, including pharmaceutical sciences, forensic and environmental analyses. The present work concentrates on the developing of new eco - friendly procedures for determination of two selected antibiotic medicaments namely cirprofloxacin chloride (CIPRO) and norfloxacin (NOR) using iron (III) ion in human serums and pharmaceutical formulations, as well as the exploitation of these two drugs in chemical analysis as chelating agents for the detection of iron in pharmaceutical formulations via using cloud point extraction coupled with molecular spectrophometry. Generally, these methods implicate the use of a nonionic surfactant (Triton X - 114) as an extracting medium which entrap the hydrophobic colored complex formed between one of these drugs and iron (III) ion in acidic medium as a reaction system for designing the CPE procedures.This thesis includes three main chapters as follows;Chapter One summarizes some theoretical and practical principles of cloud point extraction (CPE) methods and then highlights the knowledge of the target analytes (CIPRO, NOR and iron) in term of their structures, pharmacological importance besides a concise chemical literature review for the estimation of these analytes by different analytical techniques. Chapter Two consists of an outline of instrumental techniques , general apparatus and chemicals used in the present work. The full analytical procedures for CPE which have been designed for the determination of the target analytes under study are made in this thesis.Chapter Three covers a detailed study for the discussion of the analytical data obtained throughout this work which can be summed up as follows;A. Formation of chelates between CIPRO or NOR and Fe(III) in acidic medium , where the drugs have individually been estimated in the resulting complex by spectrophotometry after the cloud point extraction at each respective ?max, and the use of developed method so that to determine any of the interested drug in human serum and pharmaceuticals. At first, the study was conducted to pinpoint the optimum conditions for the formation of complexes by CPE and the results were as follows; 1. The optimum experimental conditions for Fe - CIPRO and Fe - NOR complex for the determination of CIPRO and NOR respectively : H2SO4 concentration (5x10 - 4 M and 2.5x10 - 4M; Fe(III) concentration ( 6 ?g mL - 1 and 10 ?g mL - 1); Triton X - 114 amount ( 1%) for both drugs; temperature and time ( 75 °C at 25 min and 65 °C at 20 min).2. The achieved analytical figures of merit on applying the developed methods for CIPRO and NOR are : linear range (2.5 - 120 ?g mL - 1 ) for drugs, limit of detection (0.770 and 0.204 ?g mL - 1), Enrichment factor (143 and 280 fold), extraction efficiency (96.46 and 96.62%) and mean recovery percentage (98.89±0.87% and 98.95±1.09). 3. The newly established procedures have been applied for the determination of CIPRO and NOR in human blood serum and pharmaceuticals. For the determination of these medicaments in serum samples , the statistical paired t - test was used to test the significance of the proposed method comparing with the conventional UV - spectrophotometry, while in pharmaceuticals, the findings were compared statistically with quoted values that stated by the manufactures. B. Iron (III) ion was also determined in the pharmaceutical formulations based on the above reaction system in (A) via formation of yellow colored complexes with each medicament which extracted by micelles generated by CPE and subsequently detected spectrophotometrically at the same ?max of the above mentioned complexes. The optimum established conditions and the analytical data obtained could be summarized as follows : 1. The same optimum conditions were used in (A) except that the concentration of CIPRO or NOR here was of 7x10 - 5 M and Triton X - 114 amount of 0.6% in final solutions.2. The analytical figures of merit obtained on applying the developed methods for iron using CIPRO and NOR respectively; linear range (5 - 150 ng mL - 1); limit of detection (2.67 and 3.42 ng mL - 1); preconcentration factor (71 and 83 fold); mean recovery percentage (99.78±0.53% and 98.77±2.29); extraction efficiency (99 and 98.7%). 3. The effect of some additives of the pharmaceutical formulations was also studied and the iron determined in three selected formulations collected from local drugstores. The results were compared statistically with quoted values and shown not to be significant at 95% confidence level.
