الفهرس 
General Introduction
Materials and InstrumentsOnly 14 pages are availabe for public view
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Abstract
The thesis deals with the analysis of some pharmaceuticals in pure and dosage forms using chromatographic techniques.The thesis begins with abstract and clarification of the aim of the study, as well as a special section for literary survey and comparison with previous works, then consists of three parts:
Part I:
` This part is a general introduction to separation methods using modern chromatography and is divided into two sections. The first of them deals with talking about chromatography, its meaning in general, and its importance in various fields, as well as its different classification that has developed over time.This section also deals with special attention to high performance liquid chromatography (HPLC) in terms of its features and components of the devices used (pumps, separation columns and detectors), as well as the types of liquids and solvents used and others. Finally, the basic terms, concepts and factors affecting the separation processes using high performance liquid chromatography.
The second section deals with general principles for analytical method development and validation.
Talking about a strategy for developing methods of analysis and the necessary steps for that in terms of collecting information about the sample and researching accurately to determine the goal and then specifying the requirements for analysis and choosing the appropriate conditions for the separation process and preparation of samples.
Then discuss the validation of the analytical method and its various characteristics with a comparison of the different point of view between several guidelines and how to apply it.
Part II:
This part deals with the development and validation of quantitative (HPLC-UV) analytical methods used to analyses three selected pharmaceuticals in pure and dosage forms.
This part consists of three sections.
Section one discusses a simple, and sensitive HPLC-UV method for the analysis of Etoricoxib in Ricoxitib tablets. Effective chromatographic separation was achieved using Phenomenex-Luna C18 – (150X4.6mm, 5μm) with isocratic elution of the mobile phase consisting of 0.01 M potassium dihydrogen phosphate solution in water (1.36g/L, adjusted to pH 3.5 using orthophosphoric acid): Acetonitrile: Methanol (40:15:45 v/v/v). The wavelength of detection was set to be 235 nm (UV detector), and a flow rate of 1.0 ml/min. was employed, 10 μl was used as injection volume and the column temperature was maintained at 30°C. Under these chromatographic conditions, Peak of etoricoxib was obtained at Retention time about 5.1 min. and Run time of about 7.0 minutes. The developed method was validated according to ICH guidelines for validation of analytical procedures, and successfully used.
Section two discusses a rapid, simple, and sensitive HPLC-UV method for the Brexpiprazole in Rexozolex tablets. Effective simple chromatographic separation was achieved using Phenomenex-Luna C18 – (250X4.6mm, 5μm) with isocratic elution of the mobile phase consisting of 0.5% Acetic acid glacial solution in water (5ml/L, pH about 2.85): Acetonitrile (60: 40 v/v). The wavelength of detection was set to be 315 nm (UV detector), and a flow rate of 0.8 ml/min. was employed, 20 μl was used as injection volume and the column temperature was maintained at 30°C. Under these chromatographic conditions, Peak of brexpiprazole was obtained at Retention time about 2.6 min. and Run time of about 4.0 minutes. The developed method was validated according to ICH guidelines for validation of analytical procedures, and successfully used.
Section three discusses a rapid, simple, and sensitive HPLC-UV method for the Vonoprazan in Vondalous tablets. Effective chromatographic separation was achieved using Agilent 5 HC C18 – (150X4.6mm, 5μm) with isocratic elution of the mobile phase consisting of Buffer (0.01M potassium dihydrogen phosphate (1.36 g/L) and 0.02M sodium dihydrogen phosphate (2.4 g/L) in 900ml water, adjust pH 6.8 by 5N sodium hydroxide solution then complete till 1000 ml by water): Acetonitrile (65: 35 v/v). The wavelength of detection was set to be 225 nm (UV detector), and a flow rate of 1.0 ml/min. was employed, 30 μl was used as injection volume and the column temperature was maintained at 35°C. Under these chromatographic conditions, Peak of Vonoprazan was obtained at Retention time about 3.3 min. and Run time of about 6.0 minutes. The developed method was validated according to ICH guidelines for validation of analytical procedures, and successfully used.
Part III:
This part deals with practical applications for different samples that contain the active substance in pure form and pharmaceutical preparations with different concentrations and different manufacturing sites, using the previous methods that were developed and validated for analysis. This method has been successfully used in either the quality control testing or the stability testing of the selected pharmaceutical formulations, brand product, and pure raw material.
This part is divided into three sections, each section contains all data related to the samples used, their types and characteristics. They also contain all the raw data obtained from the analysis, as well as all the results of the analysis of the percentage of assay and organic impurities of the samples.
The arrangement of these sections is as follows:
The first section, application of etoricoxib analytical method, the second section, application of brexpiprazole analytical method, and the third section, application of vonoprazan analytical method.