الفهرس 
IntroductionOnly 14 pages are availabe for public view
 |  | from | 142 |  |  |
| | | from | 142 | | |
Abstract
Summary
Chapter I
Contain the introduction which includes two parts: The first part gives an idea about Pharmaceutical drugs under investigation and there definition, structure, classification, IUPAC name, formula, molar mass and mechanism of action of this group of drugs. Also, chemical structure and physical properties.
The second part Contain the literature survey of the previous studies for the analysis methods of the studied drugs including spectrophotometric, chromatographic, colorimetric, flurometric, chemilumininse, electroanalyticaland other methods.
Chapter II
Contain the experimental part which includes apparatus used for measurement and procedures for the preparation of the solution of drugs and reagents. Also, contain the accuracy and presentation and the analytical application of both Voltammetric and spectrophotometric Methods.
Chapter III
Contain the result and discussion which include two parts:
- The first part: includes The Electroanalatical methods procedures for determination of the studied drugs (OND and TRO) behaviors using voltammetric methods in buffer solutions as supporting electrolyte at different electrodes. These electrodes are activated carbon paste electrode (CPE) and (MWCNT) in which can give the best results for determination by using (CV, DPV and SWV) techniques. The shape of the peak and its position as the peak potential (Ep) and current peak (ip) are affected by different factors such as:
- The type of buffer solution used as supporting electrode
- The pH value of the buffer solution used as supporting electrode.
- The scan rate.
The supporting electrode plays an important role in the electrochemical response its choice can modify the thermodynamics and kinetic of electrochemical processes, as well as the mass transfer within the cell.
The pH of the electrolyte medium is one of the variables that commonly and strongly influence the shape of the voltammogram, and therefore it was important to investigate the effect of pH on the electrochemical behaviour of the drugs.
-The second part: includes spectrophotometric procedures for determination of the studied drugs using:
- Zero order spectrophotometric method.
- Method-D1 (first derivative spectrophotometric method).
- Method-RD1 (first derivative of the ratio spectra).
ME and PD possess no good aqueous solubility and showed good UV absorption in methanol, thus methanol has been selected as solvent for the present analytical methods.
In the first order derivative method, aliquots of ME and PD standard stock solutions were accurately transferred in to 10 ml volumetric flasks, separately and volumes were completed with methanol. All the solutions were scanned from (200-400) nm in the spectrum mode. Thus obtained absorption spectra were derivatizedfrom first to fourth order.
First order derivative (n = 1.0) spectra showed good sensitivity and linearity hence the zero crossing wavelengths, 271 nm and 330 nm of first order derivative spectra were selected for analysis of ME and PD respectively.
The calibration curves were constructed and the concentration of individual drug present in the mixture was determined against calibration curve in quantitation mode.
Previously scanned absorption spectra of ME solutions prepared at different concentrations (1.5-20 μg/ml) in its binary mixture with PD was divided by the spectrum of the standard solution of PD (26 μg/ml) in Methanol to get the ratio spectra of ME the first derivative of the ratio spectra were than calculated. The amount of ME was determined by measuring the first derivative signal at 271 nm. A similar procedure was followed for different concentrations of PD (3.5-26 μg/ml) with ME and for division spectrum of the standard solution of ME.HCL (20 μg/ml) in methanol was used. Similarly, content of PD was determined by measuring the first derivative signal at 330 nm.
Therefore, to select most appropriate wavelength, ME was determined form the laboratory mixture at all the four wavelength and mean recovery and standard deviation were calculated and found to be 101±2.45, 100.89±1.48, 99.81±2.68 and 100.67±0.73 at 222.1, 248.2, 265.0 and 330.0 nm respectively. These points were tested for the determination of PD from the binary mixture. The synthetic mixture mean recovery of PD and standard deviation were found to be 99.5±1.06 and 101.85±1.92 at 240.9 and 270.7 nm respectively.
The proposed methods were validated as per ICH guideline and the limit of detection (LOD) and limit of quantization (LOQ) for method D1 and method RD1 for both the drugs were calculated.