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العنوان
Utility of Variable Analytical Methods for Micro Determination of Some Antidepressant /
المؤلف
Mohammad, Emam Ahmed Ali.
هيئة الاعداد
باحث / Emam Ahmed Ali Mohammad
مشرف / Mohamed .F. El-Shahat
مشرف / Alaa .S. Amin
مشرف / Ahmed.M. Adawi
مشرف / Ibrahim.H.A.Badr
تاريخ النشر
2016.
عدد الصفحات
243 p. :
اللغة
الإنجليزية
الدرجة
الدكتوراه
التخصص
Analytical Chemistry
تاريخ الإجازة
1/1/2016
مكان الإجازة
جامعة عين شمس - كلية العلوم - Chemistry
الفهرس
Only 14 pages are availabe for public view

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from 243

Abstract

The thesis comprises four chapters:
Chapter (1)
It includes an introduction concerning the theoretical bases of the pharmaceutical analysis for quality control, the research studies, spectrophotometric determinations and thin layer chromatography. Also it includes an introduction about Toxicity of Heavy metals, methods for determine metal ions and important of chemical sensors.
Chapter (2)
This chapter comprises a literature survey covering the different methods utilized for the determination of Tramadol hydrochloride (TD), Mianserin hydrochloride (MIN), Fluoxetine hydrochloride (FLU), Clomipramine hydrochloride (CLO) and Dothiepin (Dosulepin) hydrochloride (DO). These include spectrophotometric, chromatographic, electrochemical and other miscellaneous methods.
Chapter (3)
It includes the experimental part, materials, reagents, preparation of solutions and instruments. Also, this chapter includes the optimum experimental conditions for the determination of these drugs and applications to the analysis of TD, MIN, FLU, CLO and DO in pure form, formulated tablets and spiked human urine. Also, this chapter includes the experimental for thin layer chromatography (TLC) method involving, materials, and reagents, preparation of solutions, instruments and general procedure for the determination of these drugs. Also It includes the experimental part for determination of Tramadol hydrochloride and Clomipramine hydrochloride by Second Derivative Spectrophotometric method ,materials, instruments, preparation of working standard solutions, wavelength selection, and calibration curve of standard tow drugs, determination of TD and CLO in tablets and in spiked urine samples.
Also it includes the experimental part for Colorimetric determination of some toxic metal ions in post-mortem biological samples, materials, reagents, preparation of mesoporous TiO2 and instruments. Also, characterization of TiO2 sensor. Applications of this technique performed to the analysis of Cu (II), Pb (II), Hg (II) and Cd (II) ions in post-mortem blood and viscera.
Chapter (4)
It deals with the results and discussion which comprises four parts:
Part 1: Visible spectrophotometric methods
In this part, visible spectrophotometric methods have been produced for the determination of TD, MIN, FLU, CLO and DO in pure drugs, tablets and in some biological fluids.
I. The drugs were allowed to react with the PHR, CR, BCG, MY, MO and BTB. At the optimum conditions for the formation of highly colored ion-associates which are extracted with organic solvents followed by spectrophotometric measurements at λmax.
II. Studies on the effect of pH, the extraction solvents, time, temperature and interferences are performed to set up the optimum experimental conditions for the formation of ion-associates.
III. Examinations are completed to give further insight to the stoichiometric composition of the formed ion-associates. The outcomes results demonstrated that the existence of 1:1 in case of CR and MY and found 2:1 in MO with TD, 1:1 in case of CR,BCG and MY and found 2:1 in MO with MIN, 1:1 in case of BCG, PHR ,BTB and MY with FLU , 1:1 in case of BCG, PhR and MY and found 2:1 in MO with CLO and 1:1 incase of PhR and MY and found 2:1 in CR with DO.
IV. The ion-associates are utilized for analytical determination of these drugs in pure solutions, in doses form and in urine samples.
V. The got results were treated statistically and compared with those obtained by the pharmacopeia methods for estimation of the precision and accuracy. Therefore, the present methods are favorable for the drugs determination.
Part 2: Thin layer chromatography methods
In this part, the detection of TD, MIN, FLU, CLO and DO by TLC have been produced.
I. Examines on the impact of the polarity of the TLC plate (constant and high), the polarity of the development solvent (can be varied by using different solvents) and the polarity of the compounds in the spot solvents on Rf values.
II. The obtained results were as follows:
TD, DOT, MIN was TLC chromatography using systems TA, TH and TL which are appropriate for separation where gives higher RF values than other systems.
TD, FLU and DOT was TLC chromatography using systems TA, TE and TL which are the most appropriate separation where gives higher RF values than other systems.
FLU, DOT and MIN was TLC chromatography using systems TC, TE and TL which are the most reasonable for separation where gives higher RF values than other systems.
CLO, DOT and MIN was TLC chromatography using systems TA, TC and TAE which are the most suitable for separation where gives higher RF values than other systems.
III. The investigated drugs were chromatographed using the above systems, were visualized under UV light and confirmed by the colours produced with Potassium iodoplatinate and Dragendroff reagents
Part 3: Determination of Tramadol hydrochloride and Clomipramine hydrochloride by Second Derivative Spectrophotometric method
It deals with the results and discussion, Validation of the proposed method was performed. It is found that the percent recoveries were in range (97.34%- 101.34%) indicating good accuracy of the present method. The results of accuracy and precision showed that the present techniques have great repeatability and reproducibility.
Part 4 Colorometric determination of some toxic metal ions in post-mortem biological samples.
It deals with the results and discussion, in this part, visible spectrophotometric methods have been developed for the determination of Cu (II), Pb (II), Hg (II) and Cd (II) ions in post-mortem blood and viscera.
The method is depends on developed a single-step detection and removal for metal ions based on dithizone (DZ) anchored on mesoporous TiO2 with fast colorometric response and high selectivity for the first time.
Studies on the effect of pH, the amount of sensor, influence of foreign ions and reversible metals ion- sensing systems.
The obtained results were treated statistically for estimation of the precision and accuracy. The results contrasted with those got by the official method. Therefore, the present methods are suitable for the metals ion determination, as being accurate and precise to a good extent.