الفهرس | Only 14 pages are availabe for public view |
Abstract This thesis comprises five main parts: Part I: This part conains an introduction about the pharmacological action of the β-adrenergic blocking drugs. It also contains information about their therapeutic indications, mechanism of action and chemical structure of β-adrenergic blocking drugs. This part also comprises a literature review of the official and reported methods used for the determination of the studied drugs. Part II: This part describes the developement of a simple, rapid, accurate and sensitive colorimetric method for the assay of Acl, Mtl, Prl and Tml in bulk powders and in their pharmaceutical preparations. The proposed method depends on the reaction of each drug with mercurochrome in presence of citric acid phosphate buffer (pH 6.0-6.5) to form co-ordinating complexes, which can be measured spectrophotometrically in the range of 565-580 nm. The different factors that may affect the reaction such as pH, buffer volume, mercurochrome concentration, reaction time and stability of the formed product were optimized. A linear relationship 167 Summary and conclusion between the absorbance and the concentration occurred within the range 4 – 70 μg/ml. The mole ratio of mercurochrome to each of the tested drug is 1:1. The developed method was applied successfully for the determination of studied drugs in their pharmaceutical formulations. The results obtained validated by means of t-test and F-test at 95% confidence limit, no significant difference found indicating good accuracy and precision of the proposed methods. No interference observed from commonly encountered excipients. Part III: This part deals with the analysis of each of Acl, Mtl, Prl and Tml in bulk powders and in their dosage forms. The method depends on the reaction of the cited drugs with ECR (anionic dye) to form a highly colored ion-pair complex extractable in chloroform. Then the absorption intensity of the organic phase was measured at 462 nm. The reaction conditions of the method carefully studied to achieve maximum stability and sensitivity. Beer’s law was obeyed in the range 2 25 μg/ml and the mole ratios of the formed complexes were determined and found to be 2:1 (drug-ECR). The developed methods applied successfully for the determination of studied drugs in their pharmaceutical formulations. The results obtained validated by means of t-test and F-test at 95% confidence limit, no significant difference was 168 Summary and conclusion found indicating good accuracy and precision of the proposed methods. No interference observed from commonly encountered excipients. Part IV: In this part, non-extractive spectrophotometric method was described for the analysis of Acl, Mtl, Prl and Tml in bulk powders and in their dosage forms. The method depends on the reaction of the cited drugs with CRS to form a highly colored ion-pair complex measured in chloroform at 515 nm without extractions. Optimal conditions for color formation were determined for this method. Beer’s law was obeyed in the range of 1 - 12 μg/ml. The mole ratios of the formed complexes were determined and found to be 2:1 (drug-CRS). The developed method applied successfully for the determination of studied drugs in their pharmaceutical formulations. The results obtained validated by means of t-test and F-test at 95% confidence limit, no significant difference was found indicating good accuracy and precision of the proposed methods. No interference was observed from commonly encountered excipients. Part V: This part describes a sensitive method for the determination of Acl, Mtl, Prl and Tml in pure forms and or dosage forms. The method depends on the interaction of the cited drugs with acetaldehyde to form N-alkylvinylamine (enamine) which then 169 Summary and conclusion allowed to react with bromanil to give a highly colored vinylamino-substituted quinone measured spectrophotometrically at 680 nm. The reaction parameters carefully studied to obtain the optimum conditions. Beer’s law was obeyed in the range of 10 – 200 μg/ml. The developed method applied successfully for the determination of studied drugs in their pharmaceutical formulations. The results obtained validated by means of t-test and F-test at 95% confidence limit, no significant difference was found indicating good accuracy and precision of the proposed method. No interference observed from commonly encountered excipients. |