الفهرس 
Experimental ParametersOnly 14 pages are availabe for public view
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Abstract
This thesis is devoted for developing new methods for the analysis of certain quinoline; isoquinoline; and 4-quinolone derivatives of pharmaceutical interest; namely: oxamniquine, praziquantel, sparfloxacin, oxolonic acid, flumequine, enrofloxacin, fleroxacin , ciprofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate , either per se or in formulations and biological fluids. All the conditions of the proposed procedures as well as the experimental parameters are studied, discussed and explained. Furthermore the data given are statistically analyzed and compared with those obtained by compendial methods or published ones. br The thesis involves five main parts : br Part I : This part presents a survey on the structure-activity relationship of the studied quinolines and their analogues antibacterial agents; their mechanism of action, fate, absorption, excretion and bioavailability. br This part also includes a literature review covering the official methods of analysis of these compounds in addition to the previously published ones. The review describes also the reported techniques for the analysis of these compounds in dosage forms and in biological fluids. br Part II-A:This part is devoted for devolping a sensitive fluorimetric method for determination of oxamniquine, based on conversion of the drug to its nitroso derivative by Zn7CaCl2. The formed nitroso derivative is then allowed in turn to react with 2-cyanoacetamide to produce a highly fluorescent condensation product which emites a strong fluorescence at 450 nm after excitation at 370 nm, respectively. This allowed the determination of 0.08-0.88 ixg.ml”1 of oxamniquine applied to pure br samples or pharmaceutical preparations with a minimum detectability (S/N=2) of8ng.ml”\ br Part II-B-: In this part a sensitive fluorimetric assay of sparfloxacin is developed. The studied drug forms a ternary-complex with Al3+ and SDS at pH 8.3 with good stability. The emitted fluorescence can be measured at 500 nm with excitation at 310 nm. Also, sparfloxacin was measured by direct fluorimetery using acetonitrile as solvent, these two methods were applied for the quantitative analysis of the drug in its dosage forms and spiked urine and plasma samples. Also this part describes the complexation reaction of other studied 4-quinolones namely; oxolonic acid , flumequine and enrofloxacin through complex formation with Al + in an attempt to develop a fluorimetric method for the determination of these compounds either in biological fluids or in pharmaceutical preparations. br Part HI-A- :This part is concerned with studying the polarographic behaviour of certain 4-quinolones namely; enrofloxacin, sparfloxacin and fleroxacin in Britton Robbinson buffers. A well-defined cathodic wave is produced over the pH range 3.2-11.98. The wave was characterized as being irreversible,diffusion controlled with limited adsorption properties. br These findings favour a quantitative estimation of these drugs by differential pulse polarography (DPP), either in bulk, in pharmaceutical preprations or in biological fluids over the concentration range 4x 10”5 -5xl0”4 M, 2xl0~5-2xl0”4M and lxlO’5 - 4xlO”4 M using DC, mode for enrofloxacin, sparfloxacin and fleroxacin respectively and lxl0”6-4xl0° M, lxl0~6-lxl0’4 M and 2xl0’6-8xl0’5 M using DPP mode for enrofloxacin, sparfloxacin and fleroxacin respectively, with a minimum detectability (S/N—3) of ixlO”7 M for enrofloxacin , sparfloxacin and 2x10”’ M for fleroxacin respectively. br Part III-B-: This part involves a polarographic study of DQ , DPP and AC in -#111;-#114;-#100;-#101;-#114; to obtain the appropriate conditions for quantitative estimation of praziquantel in pharmaceuticals and biological fluids. br DCt, DPP and AC modes are applied over the concentration range 8-48,3.2-38.4, 0.48-20 fig. ml”1 using the three modes respectively with a minimum detectability (S/N=2) 0.02 jag. misusing AC mode. br Part-IV-A-: In this part the reaction between oxamniquine and potassium permanganate in an alkaline medium was carefully kinetically studied at room temperature for a fixed time of 20 min. The absorbance of the coloured manganate ions was measured at 610 nm. Alternatively, the decrease in the absorbance of potassium permanganate after addition of the drug was measured at 525 nm. The absorbance concentration plots in both procedures was rectilinear over the range 0.5-4 ng.ml”1. The fixed time method of 20 min was further applied to spiked urine and plasma, the parcentage recoveries were 100.94+ 0.57 and 98.07 + 0.88 for spiked urine and plasma respectively at 610 nm, and 97.51 + 1.27 and 95.69 + 1.23 for spiked urine and plasma respectively at 525 nm. br Part-IV-B-: This part is devoted for developing a simple selective kinetic procedure for the determination of certain 4-quinolones namely; norlloxacin (NFX), ofloxacin (OFX), enrofloxacin (EFX), fleroxacin (FLX) , ciprofloxacin (CFX) and pefloxacin (PFX). The procedure is based on reacting the studied compounds with 3-methyl-2-benzothiazolinone hydrazone hydrochloride (MBTH) in presence of cerium (IV) ammonium sulphate as an oxidant at room temperature for a fixed time of 20 min, for (NFX), (EFX), 12 min for (OFX) and 30 min. for FLX, CFX and PFX , then the absorbance of the reaction product is measured at 630 nm. This method was further applied to the br determination of the studied compounds either per se or in naceutical preparations. Part V : This part describes the instruments, materials, reagents and procedures.