الفهرس 
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Abstract
The Thesis Presents Three Parts, For Quantitative Determination Of Some Pharmaceutical Compounds Containing Nitrogen Atom In Their Pure And Pharmaceutical Formulations With Different Validated Methods Of Analysis.
PART І: QUANTITATIVE DETERMINATION OF PHENIRAMINE MALEATE AND ITS TOXIC IMPURITY A, IN BULK AND PHARMACEUTICAL FORMULATION.
Part I Aimed To Develop An Accurate, High Sensitive And selective Analytical Methods For Simultaneous Determination Of Pheniramine Maleate And Its Toxic Impurity A, 2- Benzyl Pyridine In Pure Drugs Forms And Its Injection Formulation.
Including Four Sections:
Section A: Introduction And Literature Review
Section A Presents A Simple Introduction About The Pharmacological Actions Of Pheniramine Maleate And Its Impurity A, 2-Benzyl Pyridine, The Chemical Structures, Physical Properties Of The Two Components, And The Literature Review Of The Previous Published Analysis Methods Of The Components Alone Or In Combination With Others.
Section B: Quantitative Determination Of Pheniramine Maleate And Its Main Toxic Impurity, 2-Benzyl Pyridine By Different Spectrophotometric Methods
Section B, Presents Different Validated, Simple And Accurate Spectrophotometric Methods Such As, Derivative Ratio Spectrophotometric Methods, Dual Wavelength Method And Ratio Difference Which Are Established For The Simultaneous Determination Of Pheniramine Maleate And Its Toxic Impurity A, 2-Benzyl Pyridine By Applying The Methods In Pure Forms And Pharmaceutical Formulations.
Section C: Green TLC-Densitometric Method For Separation And Simultaneous Determination Of Pheniramine Maleate And Its Toxic Impurity 2-Benzyl Pyridine.
This Section Provides A Green TLC-Densitometric Validated Method Which Is Simple, High Sensitive And selective For Simultaneous Determination Of Pheniramine Maleate With Its Toxic Impurity A, 2-Benzyl Pyridine. The Method Depends On The Difference Of The Resulted Drugs Peaks In Their Rf Values. The Development Was Operated In A chromatographic Tank Containing Mobile Phase Of Ethanol: Ethyl Acetate: Ammonia (8: 2: 0.1; By Volume) At Room Temperature. Then The Developed Plates Were Allowed For Air Drying For Few Minutes And Scanned At 265 Nm.
Section D: Green RP-UPLC Method For Separation And Simultaneous Determination Of Pheniramine Maleate And Its Toxic Impurity A, 2-Benzyl Pyridine.
The Section Presents A Validated, Precise, And Sensitive Green UPLC Method For Simultaneous Determination Of Pheniramine Maleate With Its Toxic Impurity A, 2- Benzyl Pyridine In Its Pure Form And Pharmaceutical Formulations.
The chromatographic UPLC Separation Was Operated At Room Temperature Utilizing A Mobile Phase Consisting Of Methanol: Water (60: 40 V/V). The Flow Rate Was 0.1 Ml/Min. The Injection Volume Was 5 Μl With Photodiode Array Detector Adjusted At 230 Nm. Successful Separation Between PAM And BNZ Compounds Was Achieved Within 4 Min.
PART П: QUANTITATIVE DETERMINATION OF OMEPRAZOLE, ASPIRIN, AND ITS IMPURITY SALICYLIC ACIC IN BULK AND PHARAMACEUTICAL FORMULATION
This Part Presents A Simple And Precise Spectrophotometric And chromatographic Analytical Methods Developed For The Simultaneous Determination Of Omeprazole, Aspirin, And Salicylic Acid In Their Pure Forms And In Their Pharmaceutical Formulation Form.
This Part Includes Four Sections:
Section A: Introduction And Literature Review
This Section Presents Summary Of The Pharmacological Actions, The Chemical Structures, And The Physical Properties Of Omeprazole, Aspirin, And Salicylic Acid. Also Brief Summary Of The Previous Published Analytical Methods For Their Determination And Analysis.
Section B: Quantitative Determination Of Omeprazole, Aspirin And Salicylic Acid By Different Spectrophotometric Methods.
This Section Aimed To Estimate Accurate And Sensitive Spectrophotometric Methods For Quantitative Determination Of OME, ASP And SA In Pure Form And In Their Pharmaceutical Formulation. The Applied Methods Were Second Derivative Spectrophotometric Spectra, First Derivative Of Ratio Spectra And Double Divisor Derivative Ratio Spectra Of First And Second Derivative Methods.
Section C: Simultaneous Determination Of Omeprazole, Aspirin And Aspirin Main Impurity, Salicylic Acid By Green Thin Layer Method (TLC)
This Part Presents Sensitive And selective Methods For OME, ASP And SA Determination In Their Bulk Powders And Dosage Formulations, Regarding To The Difference In Their Rf Values. Suitable Green Mobile Phase Has Been Used To Achieve The Optimum Separation; Also Other Necessary Parameters And Conditions Have Been Investigated.
The Separation Of The Studied Components Was Applied On 20 × 10 Cm TLC Aluminum Sheets With A Mobile Phase Of Ethanol: Ethyl Acetate (2: 8, V/V) Saturated On The chromatographic Tank For 20 Min At Room Temperature. The Applications Of The Bands Were 20 Mm Apart And 15 Mm Away from The Bottom. Linear Ascending Development Was Then Initiated. The Developed Plates Were Exposed To Air For Drying For A Few Minutes Before Scanning At 240 Nm Under The Specified Instrumental Conditions.
Section D: Green RP-UPLC Method For Separation And Simultaneous Determination Of Omeprazole, Aspirin, And Its Main Impurity Salicylic Acid
In The Presented Section, A Precise And selective RP-UPLC Method Has Been Developed And Validated For The Simultaneous Determination Of Omeprazole, Aspirin And Aspirin Main And Toxic Impurity, Salicylic Acid In Their Pure Forms And Their Pharmaceutical Formulations.
The chromatographic Isocratic Separation Was On ACQUITY UPLC® BEH C18 1.7 µm 2.1 × 150 Mm Column, With A Mobile Phase Consisting Of Ethanol: 0.1% Aqueous Solution Of Triethylamine, Ph= 3 By Orthophosphoric Acid (30: 70 V/V), At 230 Nm At Room Temperature. Adjusting Flow Rate At 0.15 Ml/Min., The Injection Volume Was 5 Μl And Photodiode Array Detector Was Used. The Separation Was Successfully Achieved With Elution Within 8 Min.
PART Ш: QUANTITATIVE DETERMINATION OF CINNARIZINE AND NICERGOLINE IN PRESENCE OF CINNARIZINE IMPURITY A, AND NICERGOLINE DEGRADATION PRODUCT IN BULK AND PHARAMACEUTICAL FORMULATION
This Work Is Objected To Validate And Develop Different Analytical Methods Which Could Separate The Main Active Components Of Cinibral® Tablet (Nicergoline And Cinnarizine) In Presence Of Nicergoline Main Degradation Product And Cinnarizine Impurity. The Proposed Methods Have The Precedence In Determination Of Nicergoline And Cinnarizine With Nicergoline Degradation Product And Cinnarizine Impurity.
The Part Includes Four Different Sections:
Section A: Introduction And Literature Review
It Is Including A Brief And Simple Introduction Of The Pharmacological Actions Of Cinnarizine, Nicergoline, Cinnarizine Impurity And Nicergoline Degradation Product, And Provides The Chemical Structures And The Physical Properties Of The Four Mentioned Components. Finally A Brief Summary Of The Previous Published Analytical Methods During Their Analysis.
Section B: Quantitative Determination Of Cinnarizine, Nicergoline, Cinnarizine Impurity A, And Nicergoline Degradation Product By Different Spectrophotometric Methods
The Presented Section Is Aimed To Estimate First Different Accurate And Sensitive Spectrophotometric Methods For Quantitative Determination Of The Two Main Components In Presence Of Their Degradation Products And Impurity In Pure Form And In Their Tablet Formulation, Using Second Derivative Spectrophotometric Spectra, Double Divisor Of Ratio Spectra Spectrophotometry, And Triple Divisor Derivative Of Ratio Spectra Spectrophotometry.
Section C: Simultaneous Determination Of Cinnarizine, Nicergoline, Cinnarizine Impurity A And Nicergoline Degradation Product By Green Thin Layer (TLC) Method.
The Presented Work Provides Simultaneous Sensitive And selective Analysis Method For CIN, NIC, IMP And DEG Determination In Their Bulk Powders And Dosage Formulation, Regarding To The Difference In Their Rf Values. Suitable Green Mobile Phase Has Been Used To Achieve The Optimum Separation; Also Other Necessary Parameters And Conditions Have Been Investigated.
This Method Was Carried Out On 20 × 10 Cm TLC Aluminum Sheets. The Bands Were Applied 20 Mm Apart And 15 Mm from The Plate Bottom Edge. Linear Ascending Development Was Done In A chromatographic Tank Previously Saturated With Ethanol: Ethyl Acetate: Ammonium Chloride Buffer (3.5: 6.5: 0.5, By Volume) For 15 Min At Room Temperature. The Developed Plates Were Allowed For Air Drying And Scanned At 230 Nm Under The Specified Instrumental Conditions.
Section D: Simultaneous Determination Of Nicergoline, Cinnarizine, Nicergoline Degradation Product And Cinnarizine Impurity, By Reversed Phase High Performance Liquid chromatography
This Section Will Discuss The Determination Of Quaternary Mixture Of Cinnarizine, Nicergoline, Nicergoline Degradation Product And Cinnarizine Impurity By selective And Sensitive RP-HPLC Method. Isocratic Elution Was Alimented On ACQUITY UPLC® BEH C18 1.7 µm 2.1 × 150 Mm Column. The Used Mobile Phase Consisting Of Methanol: Acetonitrile: Sodium Dihydrogen Phosphate Buffer (60: 5: 35 By Volume Adjusted To Ph 3 By Orthophosphoric Acid). The Flow Rate Of The Mobile Phase Was Controlled To Be 1 Ml/Min And The Injection Volume Was Adjusted To Be 20 Μl. The Photodiode Array Detector Was At 225 Nm At Room Temperature. Elution With Good Separation Of The Four Compounds Was Achieved Within 5 Min.
The Presented Thesis Refers 189 References; Contains 82 Figures And 63 Tables.
It Ends With The Arabic Summary.