Eco-friendly spectrophotometric methods for determination of remdesivir and favipiravir; the recently approved antivirals for COVID-19 treatment.

Remdesivir (REM) and Favipiravir (FAV) are recently approved antivirals prescribed in severely ill COVID-19 patients. Therefore, development of new, simple, rapid, sensitive, and selective methods for analysis of such drugs in their pharmaceutical formulations will be highly advantageous. Herein, we have developed different spectrophotometric methods for analysis of the studied analytes. Method I is based on direct spectrophotometric analysis of REM and FAV in ethanol at λmax 244 and 323 nm, respectively. For simultaneous quantitation of REM and FAV, methods II-V were followed. Method II is based on derivative spectrophotometry in which REM was determined in second-order derivative spectra at 248 nm (the zero-crossing wavelength for FAV), while FAV was measured in first-order derivative spectra at 337 nm (the zero-crossing point for REM). Method III is the dual-wavelength method in which spectral intensities were subtracted at 244-207 nm for REM and at 330-400 nm for FAV. Method IV is the ratio subtraction in which ratio spectra were obtained by a suitable divisor followed by subtraction of intensities at 272-340 nm and 335-222 nm for REM and FAV, respectively. Method V is the derivative ratio method in which the obtained ratio spectra in method IV were converted to first-order derivative and then REM and FAV were recorded at 280 and 340 nm, respectively. Calibration graphs were linear in the ranges of 1-10 µg/mL for REM through all methods and 1-20 µg/mL for FAV in methods I and II, and 2-20 µg/mL by the other methods. The evolved methods were applied to pharmaceutical dosage forms of REM and FAV. All the proposed methods were further applied to human plasma samples containing both drugs with acceptable mean recoveries.

Validated stability indicating liquid chromatographic determination of ebastine in pharmaceuticals after pre column derivatization: Application to tablets and content uniformity testing.

An accurate, simple, sensitive and selective reversed phase liquid chromatographic method has been developed for the determination of ebastine in its pharmaceutical preparations. The proposed method depends on the complexation ability of the studied drug with Zn2+ ions. Reversed phase chromatography was conducted using an ODS C18 (150 × 4.6 mm id) stainless steel column at ambient temperature with UV-detection at 260 nm. A mobile phase containing 0.025%w/v Zn2+ in a mixture of (acetonitril/methanol; 1/4) and Britton Robinson buffer (65:35, v/v) adjusted to pH 4.2, has been used for the determination of ebastine at a flow rate of 1 ml/min. The calibration curve was rectilinear over the concentration range of 0.3 - 6.0 µg/ml with a detection limit (LOD) of 0.13 µg/ml, and quantification limit (LOQ) of 0.26 µg/ml. The proposed method was successfully applied for the analysis of ebastine in its dosage forms, the obtained results were favorably compared with those obtained by a comparison method. Furthermore, content uniformity testing of the studied pharmaceutical formulations was also conducted. The composition of the complex as well as its stability constant was also investigated. Moreover, the proposed method was found to be a stability indicating one and was utilized to investigate the kinetics of alkaline and ultraviolet induced degradation of the drug. The first-order rate constant and half life of the degradation products were calculated.

Validated stability-indicating spectrofluorimetric methods for the determination of ebastine in pharmaceutical preparations.

Two sensitive, selective, economic, and validated spectrofluorimetric methods were developed for the determination of ebastine (EBS) in pharmaceutical preparations depending on reaction with its tertiary amino group. Method I involves condensation of the drug with mixed anhydrides (citric and acetic anhydrides) producing a product with intense fluorescence, which was measured at 496 nm after excitation at 388 nm.Method (IIA) describes quantitative fluorescence quenching of eosin upon addition of the studied drug where the decrease in the fluorescence intensity was directly proportional to the concentration of ebastine; the fluorescence quenching was measured at 553 nm after excitation at 457 nm. This method was extended to (Method IIB) to apply first and second derivative synchronous spectrofluorimetric method (FDSFS & SDSFS) for the simultaneous analysis of EBS in presence of its alkaline, acidic, and UV degradation products.The proposed methods were successfully applied for the determination of the studied compound in its dosage forms. The results obtained were in good agreement with those obtained by a comparison method. Both methods were utilized to investigate the kinetics of the degradation of the drug.

First and second derivative synchronous fluorescence and spectrophotometric spectroscopy for the simultaneous determination of fexofenadine hydrochloride in presence of its degradation products. Application to stability studies.

Two rapid, simple, sensitive, selective and economic derivative spectrophotometric (first [D1] and second [D2]) and synchronous spectrofluorimetric (FDSFS and SDSFS) methods have been developed for the analysis of fexofenadine hydrochloride (FXD) in the presence of its different degradation products. Derivative spectrophotometry (D1) was used to measure FXD at 223 nm in the presence of its alkaline or acidic degradation products, and at 211 nm in the presence of its oxidative degradation product. Derivative spectrophotometry (D2) was used to determine FXD at 217 nm in the presence of its alkaline or acidic degradation products, and at 215 nm in the presence of its oxidative degradation product; the UV degradation product was measured at 211 nm. Synchronous spectrofluorimetry (FDSFS) was used to measure FXD in the presence of its alkaline or acidic degradation products at 406 nm, and at 367 nm in the presence of its oxidative or UV degradation products. Synchronous spectrofluorimetry (SDSFS) was applied to determine the drug at 225 nm in the presence of its alkaline, acidic, oxidative or UV degradation products. The proposed methods were successfully applied for the determination of the studied compound in its commercial tablets. The results obtained were in good agreement with those obtained by the comparison method.

Spectrofluorimetric determination of ciclopirox olamine via ternary complex with Tb(III) and EDTA.

A highly sensitive and selective spectrofluorimetric method was developed for the determination of ciclopirox olamine in raw material and in dosage forms. The proposed method is based on the formation of a ternary complex with Tb(III) in the presence of ethylenediaminetetraacetic acid. It was found that this complex manifests intense fluorescence at lambda(em) 489 and 545 nm with excitation at 295 nm. Different experimental parameters affecting the fluorescence intensity of the complex were carefully studied and incorporated into the procedure. Under the described conditions, the method is applicable over the concentration range 30-150 and 10-70 ng mL(-1) with minimum detectability of 6.7 and 0.9 ng mL(-1) at lambda(em) 489 and 545 nm, respectively. The mean percentage recovery at lambda(em) 489 and lambda(em) 545 nm ranged between 98.7 and 100.2 for the pure substance, solution, and cream. Relative error of 0.1-0.4% and RDS of up to 0.9% were estimated at lambda(em) 489 and 545 nm. A proposal of the reaction pathway is given.