الفهرس 
IntroductionOnly 14 pages are availabe for public view
 |  | from | 159 |  |  |
| | | from | 159 | | |
Abstract
The present work aims to determination of some important drugs in various matrices by the proposed simple, rapid, accurate, and sensitive methods.
The present thesis contains five chapters:
Chapter I: Introduction.
Includes
1- Lanthanide Chemistry.
2- Synthesis of lanthanide complexes.
3- A review: lanthanide complexes and their biological importance. 4- The Biological importance of lanthanide complexes.
5- Literature survey for lanthanide complexes and its applications. 6- A review of pharmaceutical quantitative analysis techniques.
7- Analytical Method Development characterizations. 8- Analytical Method Validation parameters.
9- The studied drugs (Description, IUPAC name, and physicochemical properties).
10- Literature Review, Gives a literature survey of the previous studies for the analysis of the studied drugs including UV, HPLC, HPTLC and UPLC, methods.
11- Aim of the present work.
Chapter II: Cancer antigen 125 Assessment by using Nano Optical Sensor Terbium Schiff base Complex for Early Diagnosis of Ovarian Cancer.
In this chapter, the novel thin film nano Terbium Schiff base (Tb-schiff base) complex doped in sol-gel matrix optical sensor was designed and investigated as a new simple, sensitive and precise nano-optical sensor for early diagnosis of ovarian cancer. The nano optical sensor thin film was characterized by IR, XRD, TEM, UV-VIS, and fluorescence measurements. The performance of the designed sensor is determined through monitoring the quenching of the fluorescence intensity at 545 nm by cancer antigen 125 (CA-125) after excitation at 340 nm, pH 7.2 in DMSO. The nano Tb
complex improved the sensitivity and the specificity of CA-125 as a biomarker for early diagnosis of ovarian cancer in different serum samples of the infected women. The mechanism of the interaction between the nano Tb complex and CA-125 was discussed. The remarkable quenching of the fluorescence intensity at 545 nm of nano optical sensor Tb complex thin film doped in sol-gel matrix by various concentrations of the CA-125 was successfully used as an optical sensor for the assessment of CA-125 in different serum samples of patients with ovarian cancer. The calibration plot was achieved over the concentration range 2.0 – 127 U mL-1 CA-125 with a correlation coefficient of (0.99) and detection limit of 1.45 U mL-1. This method increases the sensitivity (97.35 %) and specificity (94.29 %) of CA-125 as a biomarker for early diagnosis of ovarian cancer.
Chapter III. Favipiravir Determination by the Enhancement of the Emission of Eu+3 Optical Sensor.
The efficiency of excited-state interaction between Eu+3 and the industrial product Favipiravir (Fav) has been studied in different solvents and various pH values. High luminescence Intensity peak at 618 nm of Europium complex in DMSO was obtained without any change in solvent pH value. The photophysical properties of the Emissive Eu+3 Complex have been elucidated, the Europium was used as optical sensor for the assessment of Fav in the pharmaceutical tablets λex=365 nm with a concentration range (0.01-600) µg/mL of Fav, correlation coefficient of 0.99 and detection limit of 0.005 µg/mL.
Chapter IV. Simultaneous Determination of Avanafil and Dapoxetine in Human Plasma Using Liquid chromatography/Tandem Mass Spectrometry (LC-MS/MS) Based on Protein Precipitation Technique.
A rapid and selective LC-MS/MS method is described for the simultaneous assay of Avanafil and Dapoxetine in human plasma via protein precipitation (PP) sample preparation technique. Tadalafil was chosen as the internal standard reaching good recovery and reproducibility while diminishing the effects of the matrix. The Agilent Zorbax Eclipse XDB C18 column (4.6 × 50 mm, 1.8 µm) was used for the chromatographic separation and analysis, while 0.1% Formic acid: Acetonitrile in ratio
II
(60:40, v/v) was utilized at a flow rate of 0.5 mL/min. It was revealed that 6 min. stop time accomplished the finest separation. The assay was linear over the range of 10-6000 ng/mL for both drugs. The established bio-analytical method validation was demonstrated following US-FDA recommendations including sensitivity, selectivity, linearity, accuracy and precision. Furthermore, other validation parameters were assessed as the dilution integrity, matrix effect, carryover, and analyte stability during both short- and long-term sample processing and storage. The adopted method was efficaciously applied to a clinical study for the concurrent determination of Avanafil and Dapoxetine in human plasma.
Chapter V. Development and Validation for Molnupiravir Assessment in Bulk Powder and Pharmaceutical Formulation by RP-HPLC-UV Method.
An accurate, sensitive and selective RP-HPLC-UV method has been established for the estimation of Molnupiravir (MOL) in pure bulk powder and pharmaceutical formulation. Separation was achieved on an Inertsil C18 column, (150.0 mm x 4.6 mm,
5.0 μm) while using a mobile phase of (20 mM phosphate buffer pH 2.5: acetonitrile; 80:20, v/v%) in an isocratic mode with a flow rate 1.0 mL/min. The λmax of MOL prepared in the chosen diluent (ethanol:water in equal proportion) was found to be 230.0 nm. The constructed calibration curve was found to be linear in the concentration range of 0.2-80.0 μg/mL. The recovery % of MOL in the proposed method was 100.29%. The limit of detection (LOD) and limit of quantification (LOQ) were 0.04 μg/mL and 0.12 μg/mL; respectively. No significant interference was detected in the presence of the common pharmaceutical formulation excipients. The method was perfectly validated following the ICH recommendations. All the obtained results were statistically compared with those of the reported method and there was no significant difference. The originated method was efficaciously employed for the assessment of MOL in bulk powder and pharmaceutical formulation.