Sustainable Spectrofluorimetric Sensing Platform for Enoxaparin Estimation: Compliance With Green Chemistry and Sustainable Development Goals Safa M. Megahed, Ahmed A. Habib Luminescence, 2026 A sensitive, sustainable, and effortless turn off–on fluorescent sensor was constructed for rapid determination of the non hromophoric drug, enoxaparin sodium (ENX). Enoxaparin is an anticoagulant utilized as a blood thinner for the treatment and prophylaxis of pulmonary embolism and deep vein thrombosis. The developed sensing platform depends on the quenching of salicylate fluorescence at 410 nm after excitation at 299 nm upon addition of ferric ammonium sulfate. The ability of ENX to displace salicylate from ferric salicylate chelate leads to restoration of salicylate fluorescence. Implementation of Box–Behnken Design (BBD) helps in optimization of different experimental parameters. A linear response was attained over a range of concentrations of ENX 0.4–2.0 μg/mL (equivalent to 0.09–0.43 μM) with detection and quantitation limits of 0.1 and 0.3 μg/mL, respectively. The developed platform was successfully employed for estimation of ENX in injection dosage form with mean recovery of 100.11 ± 1.24. The environmental sustainability of this sensor was assessed using various tools for greenness, blueness, violetness, and whiteness. Furthermore, the adherence to different sustainability development goals (SDGs) was proved.
Glycerol-Based Green RP-HPLC Method for Simultaneous Determination of Methionine and Paracetamol in Pharmaceutical Tablets Ahmed Habib, Mokhtar M. Mabrouk, Marwa Fekry, Fotouh R. Mansour Chromatographia, 2023 Methionine and paracetamol are combined in dosage forms due to the ability of methionine to compensate the deficiency in glutathione in hepatic patients. In this work, an innovative simple time-saving green RP-HPLC method using glycerol as a solely green mobile phase with water for the first time was developed for the simultaneous determination of methionine and paracetamol in their standard and in Hepamol® tablets. The chromatographic conditions were optimized using factorial design with the aid of Minitab 17® Software. The method was performed on a C18 column at 38 °C, and a mobile phase consisting of glycerol and phosphate buffer (pH 2.4) (40:60, v/v), using diode array detector at 210 nm. The mixture was separated in 5 min. The developed method was validated in accordance with ICH requirement over linearity ranges of 10–90 μg/mL for both drugs, and LODs were 3.33 μg/mL for both methionine and paracetamol. Glycerol has high safety, low UV cut-off point, low flammability, and its viscosity can be manipulated when diluted with water. The procedure was compared to the reported reversed phase liquid chromatography method in the terms of their greenness with the green analytical procedure index and the analytical eco-scale. This work breaks new ground for scientists to use glycerol in greener RP-HPLC applications.
Design of experiment-oriented development of solvent-free mixed micellar chromatographic method for concomitant determination of metronidazole and ciprofloxacin hydrochloride Sherin F. Hammad, Ahmed A. Habib, Amira H. Kamal, Safa M. Megahed Scientific Reports, 2023 A green, fast and robust solvent-free chromatographic method has been developed for concomitant analysis of ciprofloxacin HCl and metronidazole in bulk powder as well as in dosage form using levofloxacin as internal standard (I.S.). Two different designs including fractional factorial (FFD) and Box–Behnken (BBD) designs were implemented for screening and optimization steps, respectively. The optimum chromatographic separation was accomplished using mobile phase composed of 0.13 M sodium dodecyl sulfate and 0.02 M Birij-35 solution adjusted to pH 2.5 using phosphoric acid at a flow rate of 1.3 mL/min and column oven temperature of 40 °C. Chromatographic analysis was performed on X-Bridge (150 mm × 4.6 mm, 5 μm) column with UV detection at 280 nm. A linear response was acquired over the range of 0.4–50 μg/mL for both drugs. The developed method was applied for quantitation of cited drugs in commercially available tablet with mean percent recovery ± SD of 99.45 ± 0.72 and 100.13 ± 0.81 for metronidazole and ciprofloxacin respectively. The method was proven to be green as evaluated by three greenness assessment tools. The run time was 8 min, thus saving time and reagent.
Quality by design paradigm for optimization of green stability indicating HPLC method for concomitant determination of fluorescein and benoxinate Amira H. Kamal, Ahmed A. Habib, Sherin F. Hammad, Safa M. Megahed Scientific Reports, 2023 A green, robust and fast stability indicating chromatographic method has been developed for concomitant analysis of fluorescein sodium and benoxinate hydrochloride in the presence of their degradation products within four minutes. Two different designs including fractional factorial and Box–Behnken designs were implemented for screening and optimization steps, respectively. The optimum chromatographic analysis was achieved using a mixture of isopropanol and 20 mM potassium dihydrogen phosphate solution (pH 3.0) in the ratio 27:73 as mobile phase. The flow rate was 1.5 mL/min and column oven temperature was 40 °C. Chromatographic analysis was performed on Eclipse plus C18 (100 mm × 4.6 mm × 3.5 μm) column with DAD detector set at 220 nm. A linear response was acquired over the range of 2.5–60 μg/mL and 1–50 μg/mL for benoxinate and fluorescein respectively. Stress degradation studies were executed under acidic, basic, and oxidative stress conditions. The method was implemented for quantitation of cited drugs in ophthalmic solution with mean percent recovery ± SD of 99.21 ± 0.74 and 99.88 ± 0.58 for benoxinate and fluorescein respectively. The proposed method is more rapid and eco-friendly compared to the reported chromatographic methods for determination of cited drugs.
Novel experimental design paradigm for development of eco-friendly gradient chromatographic method for simultaneous determination of metronidazole and spiramycin Safa M Megahed, Ahmed A. Habib, Sherin F. Hammad, Amira H. Kamal Journal of Separation Science, 2023 This work describes the innovative experimental design‐assisted development of a green gradient chromatographic method for concomitant analysis of metronidazole (MTR) and spiramycin (SPR). Two different designs including fractional factorial and Box‐Behnken designs were implemented for screening and optimization steps, respectively. The optimum chromatographic conditions involved a mobile phase consisting of ethanol and 20 mM sodium dihydrogen phosphate solution (pH adjusted to 2.5) in the ratio 2:98 (v/v) for 2 min then the ratio changed to 30:70 (v/v). The flow rate was 1.3 mL/minute. Separation and analysis were performed on X‐bridge C18 (150 mm × 4.6 mm × 3.5 μm) column with diode array detector set at 230 nm. Column oven temperature was 40°C. A linear response was acquired over the range of 5–125 μg/mL for both drugs. Detection and quantitation limits were 0.86 and 2.62 μg/mL for MTR and 0.92 and 2.83 μg/mL for SPR, respectively. The method was implemented for determination of both drugs in three tablet formulations. The method was proved to be green as evaluated by three assessment tools. The application of experimental designs assists in development of a robust green chromatographic method in gradient elution mode for determination of both drugs within reasonable time.
Green micellar stability-indicating high-performance liquid chromatography method for determination of rupatadine fumarate in the presence of its main impurity desloratadine: Oxidative degradation kinetics study Mona M. Amer, Ahmed A. Habib, Sherin F. Hammad, Amira H. Kamal Journal of Separation Science, 2023 A green micellar stability‐indicating high‐performance liquid chromatography method was developed for rupatadine fumarate determination in existence with its main impurity desloratadine. Separation was attained using Hypersil ODS column (150 × 4.6 mm, 5 μm), the micellar mobile phase consisted of 0.13 M sodium dodecyl sulfate, 0.1 M disodium hydrogen phosphate adjusted by phosphoric acid to pH 2.8 and 10% n‐butanol. The column was maintained at 45◦C and detection was carried out at 267 nm. A linear response was achieved over the range of 2–160 μg/ml for rupatadine and 0.4–8 μg/ml for desloratadine. The method was applied for rupatadine determination in alergoliber tablets and alergoliber syrup without the interference of methyl paraben and propyl paraben present as main excipients. Rupatadine fumarate revealed pronounced susceptibility to oxidation; further study of oxidative degradation kinetics was carried out. Rupatadine was found to follow pseudo‐first‐order kinetics when exposed to 10% H2O2 at 60 and 80°C and the activation energy was found to be 15.69 Kcal/mol. At a lower temperature (40°C), degradation kinetics regression was best fitted as a polynomial quadratic relationship, thus rupatadine oxidation at a lower temperature tends to adopt a second‐order kinetics rate. Oxidative degradation product structure was revealed using infrared and found to be rupatadine N‐oxide at all temperature values.
Green Assay of Tolmetin Sodium Using Solid Contact Potentiometric Sensor Doped with Ionophore and Supported with Docking Study: Application to Human Plasma and Pharmaceutical Formulations Manal F. Mahrous, Mokhtar M. Mabrouk, Ahmed Habib, Mohammed E. Draz Journal of the Electrochemical Society, 2023 Tolmetin sodium (TOL) is a non-steroidal anti-inflammatory drug used to treat arthritis. Potentiometric ion selective electrodes (ISEs) bypass sample pre-treatment, high-tech apparatus, and toxic chemicals. The current study aimed to develop and validate a potentiometric analyser for the direct assay of TOL in pharmaceutical dosage form and human plasma. We designed an experimental approach to determine the factors that affect the performance of the developed sensor. A solid contact glassy carbon electrode was utilized as a support for the developed sensor. The interaction of TOL with several ionophore was studied using molecular docking. The optimized sensor was fabricated using dioctyl phthalate as plasticizer, tetra dodecyl ammonium bromide as anion exchanger, and β cyclodextrin as ionophore.The sensor achieved −58.78 Nernstian response within 1.00 × 10−2–2.00 × 10−6 mol l−1 linear range, 1.56 × 10−6 mol l−1 LOD, and fast response within 7 s. The greenness of the proposed method was assessed using the Analytical Eco-scale and the “Green Analytical Procedure Index” (GAPI) metric tools and compared with the reported methods and gained high scores. The proposed method has several advantages in encouraging quality control and clinical labs to routinely use the developed sensor in the assay of TOL in pharmaceutical dosage forms and human plasma.
Electrochemical approach for determination of tertahydrozoline HCL using gold nanoparticles electrode Analytical and Bioanalytical Electrochemistry, 2020
Implementation of factorial design for optimization of forced degradation conditions and development of validated stability indicating RP-HPLC method for Lidocaine hydrochloride Der Pharma Chemica, 2015
