الفهرس 
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Abstract
Summary
The thesis consists of five parts
Part I: General Introduction and Literature Review
This part is divided into two sections:
Section A: Introduction.
It includes a brief idea about polyionic compounds, their classification, their properties and their presence in biological, environmental and pharmaceutical products.
Section B: Literature Review.
It includes a review of the structures, the chemical and physical properties of the studied drugs; Cromolyn sodium and Polymyxin B sulphate. Furthermore, it is concerned with different analytical methods reported in literature which aim for the determination of the chosen drugs in pure form, pharmaceutical formulations and biological fluids.
Part II: Potentiometric determinations of certain polyionic drugs
This part is divided into three sections:
Section A: Introduction to ion–selctive electrodes (ISEs).
This section describes the theory and the different types of ion selective electrodes. Also, it includes their assembly and their use with other fields.
Section B: Potentiometric determinations of Cromolyn sodium using electrochemical sensors in presence and in absence of iron oxide nanoparticles.
In this section, two graphite electrodes were fabricated using metallic mercury in sensor 1 and metallic mercury and magnetic iron oxide nanoparticles in sensor 2. Dioctyl phthalate was used as a plasticizer in a polymeric matrix of polyvinyl chloride.
The performance of the proposed electrodes was assessed according to the IUPAC recommendations and showed that they had fast, stable and nernstian response.
Response time, effect of pH and temperature on the response, selectivity and stability of the electrodes were studied to determine the optimum conditions for the determination of Cromolyn sodium in pure form, pharmaceutical formulations, and biological fluids (plasma and urine).
The sensors showed linear responses in the concentration range of 10-6 to 10-3 M and 10-8 to 10-3 M with mean percentage recoveries of pure drug (99.94 ± 0.59 and 100.60 ± 0.75) for sensors 1 and 2; respectively.
Section C: Potentiometric determinations of Polymyxin B sulphate using precipitation and ionophore based techniques.
This section describes the determination of Polymyxin B sulphate using sodium tetraphenylborate (sensor 1) and phosphotungstic acid (sensor 2) as anionic exchangers and using inclusion of the drug into β-CD cavity (sensor 3). Dioctyl phthalate was used as a plasticizer in a polymeric matrix of polyvinyl chloride.
The performance of the three electrodes was assessed according to the IUPAC recommendations and showed that they had fast, stable and nernstian response.
Response time, effect of pH and temperature on the response, selectivity and stability of the electrodes were studied to determine the optimum conditions for the determination of Polymyxin B sulphate in pure form, pharmaceutical formulations, and biological fluids (plasma and urine).
The sensors showed linear response in the concentration range of 10-6 to 10-2 M, 10-6 to 10-3 M and 10-7 to 10-4 M with mean percentage recoveries of pure drug (99.90 ± 1.55, 100.26 ± 1.15 and 100.20 ± 0.61) for sensors 1, 2 and 3; respectively.
Part III: Spectrophotometric procedures for determination of certain polyionic drugs
This part is divided into three sections:
Section A: Introduction to different spectrophotometric procedures for determination of pharmaceutical substances.
This section includes the introduction of several spectrophotometric procedures that were applied in the analytical studies of pharmaceutical substances.
Section B: Zero order, H-point standard addition method and area under the curve determinations of Cromolyn sodium in presence of Oxymetazoline HCl.
In Zero order method, Cromolyn sodium was measured at 327.0 nm. Absorbances were recorded at 241.5 nm and 274.9 nm for H-point standard addition method and the wavelength was selected in ranges 232.0 - 254.0 nm and 216.0 - 229.0 nm for area under the curve method.
These methods were applied for determination of Cromolyn sodium in presence of Oxymetazoline HCl in bulk powder with mean percentage recoveries (100.15 ± 0.99, 100.19 ±1.22 and 100.08 ±1.12), in laboratory prepared mixtures (100.04 ± 1.20, 100.54 ± 1.06 and 99.39 ± 1.09) and in pharmaceutical formulation (103.90 ± 0.07, 103.92 ± 0.26 and 104.15 ± 0.82), respectively.
Section C: First derivative and derivative ratio spectrophotometric determinations of Polymyxin B sulphate in presence of Oxytetracycline HCl.
The Zero crossing method has been utilized to measure the first derivative value of the derivative spectrum. Polymyxin B sulphate was measured at 219.6 nm. While for the first derivative of the ratio spectra, Polymyxin B sulphate was measured at 212.5 nm.
These methods were applied for determination of Polymyxin B sulphate in presence of Oxytetracycline HCl in bulk powder with mean percentage recoveries (100.62 ± 1.00 and 100.49 ± 1.02), in laboratory prepared mixtures (100.69 ± 1.16 and 100.93 ± 1.20) and in pharmaceutical formulation (106.17 ± 0.33 and 107.01 ± 0.21), respectively.
Part IV: Synchronous Spectrofluorimetric determinations of certain polyionic drugs
This part is divided into three sections:
Section A: Introduction to Synchronous Spectrofluorimetry.
In this section a brief introduction about the evolvement of the synchronous spectrofluorimetric technique is given, describing its advantage over conventional spectrofluorimetric technique.
Section B: Derivative synchronous spectrofluorimetric determinations of Cromolyn sodium in presence of Oxymetazoline HCl and Cromolyn sodium alkaline degradate.
The first derivative synchronous fluorescence signal was measured at 290.0 nm for determination of Cromolyn sodium in presence of Oxymetazoline HCl and the second derivative synchronous fluorescence signal was measured at 318.0 nm for determination of Cromolyn sodium in presence of Oxymetazoline HCl and Cromolyn sodium alkaline degradate, using constant wavelength difference Δλ = 145 nm.
The study of different experimental factors affecting the fluorescence intensity as constant wavelength differences, effect of pH, diluting solvents and surfactants was done.
First and second derivative synchronous spectrofluorimetry have been utilized for the determination of Cromolyn sodium in bulk powder with mean percentage recoveries (100.37 ± 0.85 and 100.09 ± 1.16), in laboratory prepared mixtures (99.74 ± 1.34 and 99.53 ± 1.46) and in pharmaceutical formulations (104.20 ± 0.58 and 104.17 ± 0.29) and (103.33 ± 0.29 and 102.50 ± 0.50), respectively.
Section C: Synchronous Spectrofluorimetric determination of Polymyxin B sulphate using Factorial Design.
In this section, different parameters affecting the reaction of NBD-Cl with Polymyxin B sulphate were investigated using the factorial design.
The studied factors included pH of borate buffer, volume of buffer, volume of NBD-Cl, temperature, time of heating and volume of concentrated H2SO4.
Synchronous fluorescence signal was measured at 440.0 nm using constant wavelength difference Δλ =80 nm.
The proposed method was successfully applied for determination of the mentioned drug with mean percentage recovery in pure form (100.23 ± 1.13) and in plasma (105.62 ± 0.36).
Part V: Chromatographic determination of Cromolyn sodium in presence of Oxymetazoline HCl and Cromolyn sodium alkaline degradate
This part is concerned with the application of isocratic high performance liquid chromatographic method for determination of Cromolyn sodium in presence of Oxymetazoline HCl and Cromolyn sodium alkaline degradate usig C18 column (250 mm x 4.6 mm x 5 μm).
The mobile phase of choice was acetonitrile:water (70:30, v/v) with a flow rate of 1.0 mL min-1 and the diode array detector was at 235.0 nm.
The proposed method was successfully applied for determination of the mentioned drug in pure form with mean percentage recovery (100.17 ± 1.04), laboratory prepared mixtures (99.82 ± 0.78) and pharmaceutical formulations (104.97 ± 0.26) and (103.96 ± 0.09).
This thesis contains 195 references, 58 tables, 57 figures and ends with Arabic