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Abstract
This thesis aimed to develop some novel potentiometric (P) and fluorimetric (F) methods for micro determination of three pharmaceutical compounds(which have a large side effects and adverse reactions with human bodies if they are exposed to it in definite amount of water) as pollutants in pharmaceutical wastewater during and after cleaning and washing different machines and tools used in industry, validation of the suggested (P) and (F) methods and comparing with standard and compendium methods.
Chapter 1: includes introduction covering biosphere, pollution types, impacts, The side effect of three different pharmaceutical compounds, an overview, including the two theoretical principles of (P) and (F) analysis methods.
Chapter 2: Presents the aim and basis of the work and literature review of the three different pharmaceutical compounds that were chosen.
Chapter 3: Presents the experimental and discussion for the methods of analysis for the three different pharmaceutical compounds were chosen. (three parts)
Part I Sensitive (F) and (P) methods are developed for the determination of gatifloxacin. The characteristic maximum emission fluorescence peak was observed for gatifloxacin at 495 nm, after its excitation at 291 nm. Concentrations in the range 16-120 ng ml-1 could be quantitated relatively rapidly by this method in pH range (4.2 - 6) with detection limit of 3.97 ng ml-1 and lower quantization limit of 13.25 ng ml-1. The (P) method exhibits the construction, evaluation and the application of a novel coated graphite rod gatifloxacin ISE. It is based on the use of the ion-associate species, formed by gatifloxacin, which was formed by gatifloxacin cation and phosphotungestate counter ion. The basic electrode performance characteristics are evaluated according to IUPAC recommendations. It exhibits a linear Nernstian response over the concentration range 9.2x10-5 to 9.2x 10-3 moll-1 solution, with a cationic slope of 28.7 ± 0.5 mV decade-1 pH range of 1.8-2.8.
Part II Includes a direct (F) method for the determination of chlorodesmethyldiazepam (C.D.D.) that was proposed. The fluorescence process was pH dependent. The linear relationship between the fluorescence intensity and concentration was with correlation coefficient r2 of 0.9958. The detection limit for the method was found to be 0.224 µg ml-1.
Part III A new clavulanate- selective electrode based on the ion-pair formed from ramipril copper II complex and clavulanate is described. The electrode, was prepared by incorporating the ion-pair into plasticized poly (vinyl chloride) PVC membrane using dioctylphthalate (DOP) as the plasticizing solvent mediator and cetyltrimethyl ammonium bromide (CTAB) as an anion excluder. The composition 1.2, 60.1, 7.7 and 31.0 mg of the ion-pair, plasticizer, (CTAB) and PVC dissolved in 6 ml of tetrahydrofuran (THF), were directly coated on the surface of a graphite disk this composition of the membrane cocktail worked well over a wide concentration range (3.5x10-5 to 7x10-2 moll-1) with a Nernstian slope of -62.3 ±0.5mV decade-1 of activity