الفهرس 
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Abstract
Five respiratory medications, (TER& BAM) quantified spectrofluorimetrically, (CHX) electrochemically (potentiometrically) and (AMB & BMH) spectrophotometrically using a variety of techniques. The submitted thesis is divided into five parts:
Part I: General introduction
This section provided a general introduction to the medications under screening. The first subsection involves mechanism of action, medicinal indications, pharmacokinetics and structural properties of the drugs under study. However, analytical review includes some of the reported methodologies for quantifying the drugs under consideration in their pharmaceutical formulations. Finally, the goal of the described thesis was completely mentioned.
Part II: Green assessment of a novel Chlorphenoxamine-selective on borate based membrane electrode: Green and Blue Profile Assessment
In the current search, an environmentally friendly novel borate based membrane electrode with unique selectivity toward cationic chlorphenoxamine hydrochloride (CHX) is reported. The sensor is based on borate as cation-exchanger and O-NPOE as a plasticizer in addition to polyurethane(PU) as a matrix .The optimized membrane sensor revealed near-Nernstian responses (59.694 mV decade-1) over (CHX) conc. range of 2.98x10 -5- 10-2 M as measured in 0.1M acetate buffer, pH 4.7.
The resulting sensor displays a selectivity pattern, with a specificity for chlorphenoxamine over other respiratory drugs (bambuterol, terbutaline), other inorganic cations (potassium, magnesium, ammonium, calcium, sodium) and other additives found in the pharmaceutical preparations (lactose, fructose, maltose, starch, talc).
The developed sensor was shown to be green and capable of determining CHX in pharmaceutical forms with high accuracy and precision. The acquired results agreed well with the standard method of (CHX) analysis. The approach’s greenness was determined utilizing analytical Eco-Scale criteria. It achieved a score of 90 in the Eco-Scale and GAPI approaches.
Part III: Solid-contact ion selective electrode using multi-walled carbon nanotubes for determination of Chlorphenoxamine hydrochloride; Green and Blue Profile Assessment
The described approach was a glassy carbon electrode (GCE) improved with (MWCNTs) was developed by casting MWCNT suspension on the surface of the GCE. Solvent evaporation from this solution produced a thick surface layer of MWCNT. The sensor is based on TFMPB as a cationic exchanger and O-NPOE as a plasticizer, as well as PVC as a matrix and CNTs to improve sensor performance.
The electrochemical reaction mechanism of chlorphenoxamine hydrochloride (CHX) was assessed at the MWCNT modified GCE (MWCNT/GCE) in 0.1 M acetate buffer solution, pH 4.7. The optimized membrane sensor was shown near-Nernstian responses (53.627 mV decade-1) over (CHX) conc. range of 2.98x10 -5 - 10-2 M.
The resulting sensor displays a selectivity pattern, with a specificity for chlorphenoxamine over other respiratory drugs ( bambuterol, terbutaline), other inorganic cations (potassium, magnesium, ammonium, calcium, sodium) and other additives included in the pharmaceutical preparations (lactose, maltose, fructose, starch, talc).
The developed sensor was shown to be green and capable of determining the tested drugs in pharmaceutical forms with high accuracy and precision. The acquired results agreed well with the standard method of (CHX) analysis. The method’s greenness was determined utilizing analytical Eco-Scale criteria. It achieved a score of 90 in the Eco-Scale, GAPI approaches, AGREE and BAGI.
Part IV: Micelle-enhanced spectrofluorimetric method for the rapid determination of bronchodilator terbutaline and its prodrug bambuterol: Application for content uniformity test
This part included a unique, easy, and sensitive spectrofluorimetric method for determining (TER) and its prodrug (BAM) in pure and pharmaceutical dose forms. The proposed method involves employing sodium dodecyl sulphate (SDS) as a micellar medium to boost the native fluorescence of either TER or BAM at 315 and 297.2 nm following excitation at 277 and 259, respectively. In the presence of 0.7% w/v SDS, the RFI of TER and BAM is increased 1.38-fold and 1.18-fold, respectively. Over the concentration range of 0.8-16 µg mL-1, the fluorescence-concentration curves were rectilinear, with LOD of 0.252 and 0.26 (µg mL-1), LOQ of 0.76 and 0.79 (µg mL-1), determination coefficients (r2) of 0.9981, and slopes of 45.92 and 10.44 for TER and BAM, respectively. The proposed method was validated in line with ICH requirements and was successfully employed in the analysis of the medications tested in their commercial tablets. The suggested approach’s high sensitivity allows it to be used to evaluate the content uniformity testing of the examined medications in their tablets utilizing the official United States Pharmacopoeia standards (USP). Statistical comparisons of the findings with those of the described techniques showed very high agreement and no significant discrepancies in precision and accuracy.
Part V: Green spectroscopic method for quantification of AMB and BMH utilizing Xanthene dye, Erythrosine B: Green and Blue Profile Evaluation.
In the current research, AMB & BMH were quantified via a green, reliable, sensitive, and non-extracting spectrophotometric approach that relied on ion-pair complexes’ formation with xanthene dye, EB. Without using any organic solvents, the pink color of the created ion-pair complexes was detected at λ = 554 nm and 556 nm for AMB and BMH, respectively. The spectrophotometric absorbance-conc. plot is straight over the ranges (1.0–8) μg/mL for AMB with LOD of 0.15μg/mL and LOQ of 0.46μg/mL and rectilinear over the ranges (1.0–9) μg/mL for BMH with LOD of 0.199μg/mL and LOQ of 0.605μg/mL. The developed technique was verified which is based on ICH criteria and employed in the examination of commercial medication formulations comprising mucolytic agents; with the findings matching those obtained using the comparison approach. Finally, the reaction ratio between (AMB & BMH) and EB was calculated utilizing Job’s approach. Depending on the study, the reaction molar ratio of (AMB & BMH) with EB was 1:1.
The yielded compounds were freely water soluble, so no need for organic solvents, making the suggested technique safer for the environment than previously described potentiometric methods.
Moreover, organic solvent extraction is not required; therefore, the generated ion-pair complexes could be directly measured. Owing to the method’s greenness and simplicity, it could be efficiently employed in quality control laboratories instead of the previously reported spectrofluorimetric and HPLC techniques.