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Two sensitive, rapid, and accurate derivative emission spectrofluorimetric methods applying zero crossing techniques were developed for simultaneous determination of binary mixtures of ibuprofen (IBU) and phenylephrine hydrochloride (PHE) in pure powder, synthetic mixture and combined tablets. The proposed methods were performed via measuring the intersected drug derivative amplitude of one drug at the zero crossing points for the other one and vice versa. The two methods rely on the measurement of the combined drugs native fluorescence after excitation at 270 nm in methanol directly, followed by differentiation using first (D 1 ) and second derivative (D 2 ) techniques. Applying the D 1 , IBU was measured quantitatively at 293.1 nm at zero crossing of PHE, on the other side; PHE was measured quantitatively at 300.7 nm at zero crossing of IBU. By the same way, applying the D 2 , the wavelengths selected were 303.5 nm for IBU and 312.9 nm for PHE. The concentration plots of derivative fluorescence intensity were rectilinear over the range of 0.5-10 μg/mL and 0.025-0.5 μg/mL for IBU and PHE, respectively. The results obtained with average % recoveries ± RSD are 99.73 ± 0.72 (IBU, D 1 ), 99.49 ± 0.95 (PHE, D 1 ), 99.79 ± 0.47 (IBU, D 2 ), and 99.88 ± 0.34 (PHE, D 2 ) were in good agreement with the comparison method. The proposed methods offer high sensitivity that enable direct analysis of IBU and PHE in spiked human plasma. The proposed methods were entirely validated in terms of ICH guidelines., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Two binary mixtures containing codeine (COD) with either ibuprofen (IBU), mixture 1, or with phenylephrine hydrochloride (PE), mixture 2, were analyzed using three simple eco-friendly spectrofluorimetric methods without the need to a prior separation step. The first method is derivative emission spectrofluorimetry using λ ex  = 236 nm and 275 nm for mixtures 1 and 2, respectively. The second method is constant-wavelength synchronous spectrofluorimetry using ∆λ = 100 nm and 60 nm for mixtures 1 and 2, respectively. The last method is constant-energy synchronous spectrofluorimetry where a wave number interval of -7000 cm -1 was used for the analysis of the two binary mixtures. All measurements were performed in acetate buffer pH 5 and thus no toxic volatile solvents were used increasing method greenness. High sensitivity was attained for the three studied drugs where the lower limits of quantitation of COD, IBU and PE reached 0.064, 0.512 and 0.087 μg/mL, respectively. Analysis of the two binary mixtures in their tablet and liquid dosage forms was performed with good accuracy and precision using the developed methods. The results of the proposed and reported methods were statistically evaluated using one-way ANOVA test and no significant difference among them was obtained. In addition, all aspects of ICH guidelines on analytical method validation were conducted., (Copyright © 2018 Elsevier B.V. All rights reserved.)

Three advanced chemmometric-assisted spectrophotometric methods namely; Concentration Residuals Augmented Classical Least Squares (CRACLS), Multivariate Curve Resolution-Alternating Least Squares (MCR-ALS) and Principal Component Analysis-Artificial Neural Networks (PCA-ANN) were developed, validated and benchmarked to PLS calibration; to resolve the severely overlapped spectra and simultaneously determine; Paracetamol (PAR), Guaifenesin (GUA) and Phenylephrine (PHE) in their ternary mixture and in presence of p-aminophenol (AP) the main degradation product and synthesis impurity of Paracetamol. The analytical performance of the proposed methods was described by percentage recoveries, root mean square error of calibration and standard error of prediction. The four multivariate calibration methods could be directly used without any preliminary separation step and successfully applied for pharmaceutical formulation analysis, showing no excipients' interference., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Resolution of binary mixtures of paracetamol, phenylephrine hydrochloride and chlorpheniramine maleate with minimum sample pre-treatment and without analyte separation has been successfully achieved by methods of partial least squares algorithm with one dependent variable, principal component regression and hybrid linear analysis. Data of analysis were obtained from UV-vis spectra of the above compounds. The method of central composite design was used in the ranges of 1-15 mg L(-1) for both calibration and validation sets. The models refinement procedure and their validation were performed by cross-validation. Figures of merit such as selectivity, sensitivity, analytical sensitivity and limit of detection were determined for all three compounds. The procedure was successfully applied to simultaneous determination of the above compounds in pharmaceutical tablets., (Copyright 2009 Elsevier B.V. All rights reserved.)