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Please use this identifier to cite or link to this item: http://hdl.handle.net/123456789/19255

Title: Kinetic Spectrophotometric Determination of Fluoroquinolones Containing Mono-substituted Piprazine
Authors: Al-Arfaj, Hessa Abdul-Rahman
Darwish, Dr. Ibrahim A
Keywords: Analytical chemistry
Pharmaceutical Chemistry
Issue Date: 29-Jun-2009
Abstract: The study described the kinetic spectrophotometric determination of four widely prescribed fluoroquinolone antibacterials containing mono-substituted piprazine in their structures. These drugs were NOR, GAT, CIP, and LOM. The kinetic spectrophotometric determination was achieved by two methods: CONDENSATION METHOD FOR DETERMINATION OF NOR AND GAT This method was based on the formation of colored N-vinyl chlorobenzoquinone derivatives of both NOR and GAT by their condensation with TCBQ in presence of ACD. The N-vinylpiprazine derivative of each drug, which formed from the interaction of the mono-substituted piprazinyl group of the drug, was subsequently condensed with TCBQ to give the colored N-vinyl chlorobenzoquinone derivative. The formation of the colored product was monitored spectrophotometrically by measuring the absorbance at 625 and 655 nm for NOR and GAT, respectively. The factors affecting the reaction was studied and optimized. The stoichiometry of the reaction was determined and the reaction pathway was postulated. The condensation reaction for both NOR and GAT was found to follow pseudo-first order. The activation energy of the reaction was calculated and found to be 5.72 and 4.15 KJ/mole for NOR and GAT, respectively. The initial rate and fixed time (at 5 min) methods were utilized for constructing the calibration graphs. In the initial rate method, the graphs were linear in concentration ranges of 10–150 and 2–120 μg/ml with LOD of 8.4 and 0.84 μg/ml for NOR and GAT, respectively. In the fixed time method, the graphs were linear in concentration ranges of 8–180 and 10–140 μg/ml with LOD of 3.2 and 3.5 μg/ml for NOR and GAT, respectively. The analytical performance of both methods was fully validated, and the results were satisfactory. No interferences were observed from the excipients that are commonly present in the pharmaceutical formulations of both NOR and GAT. As well, tinidazole that is coformulated with NOR in Conaz® tablets did not interfere with the determination of NOR. The proposed methods were successfully applied to the determination of NOR and GAT in their commercial pharmaceutical formulations of both NOR and GAT. The label claim percentages were 98.7–100.4 ± 0.68–1.03% for NOR and 98.2–100.5 ± 0.71–1.29% for GAT. Statistical comparison of the results obtained from the proposed methods with those of the official or reported methods showed excellent agreement and proved that there was no significant difference in the accuracy and precision between the proposed and the reference methods. The proposed kinetic spectrophotometric method has many advantages over many of the reported spectrophotometric methods such as procedures simplicity, short reaction time, and enhanced selectivity. These advantages encourage the application of the proposed method in routine analysis of NOR and GAT in quality control laboratories, as alternatives for the existing methods. OXIDATION METHOD FOR DETERMINATION OF CIP AND LOM This method was based on the oxidation of CIP and LOM with alkaline KMnO4 to give green colored manganate ions as reaction product. The reaction was monitored spectrophotometrically by measuring the absorbance of the reaction product at 610 nm. The factors affecting the reaction was studied and optimized. The stoichiometry of the reaction was determined and the reaction pathway was postulated. The oxidation reaction for both CIP and LOM was found to follow pseudo-first order. The activation energy of the reaction was calculated and found to be 4.48 and 4.17 KJ/mole for CIP and LOM, respectively. The initial rate and fixed time (at 5 min) methods were utilized for constructing the calibration graphs. In the initial rate method, the graphs were linear in concentration ranges of 8–100 and 2–60 μg/ml with LOD of 2.54 and 0.66 μg/ml for CIP and LOM, respectively. In the fixed time method, the graphs were linear in concentration ranges of 8–180 and 8–75 μg/ml with LOD of 3.0 and 1.3 μg/ml for CIP and LOM, respectively. The analytical performance of both methods was fully validated, and the results were satisfactory. The proposed methods were successfully applied to the determination of both CIP and LOM in their commercial pharmaceutical dosage forms. The label claim percentages were 99.4–100.2 ±1.15–1.81%. Statistical comparison of the results with those obtained by the reference methods showed excellent agreement between the accuracy and precision of the two methods. The proposed method has a great value in its application to the analysis of CIP and LOM in quality control laboratories. The proposed kinetic spectrophotometric method is superior to many visible spectrophotometric methods in terms of its simple procedures, short reaction time, high sensitivity, and wide linear dynamic range. From the economical point of view, all the analytical reagents are inexpensive, have excellent shelf life, and are available in any analytical laboratory. These advantages encourage the application of the proposed method in routine analysis of CIP and LOM in quality control laboratories, as alternatives for the existing methods
Description: Masters
URI: http://hdl.handle.net/123456789/19255
Appears in Collections:College of Pharmacy

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