A novel ecofriendly, cost and time saving high‐performance thin‐layer chromatographic method was developed and validated for simultaneous determination of metoclopramide, ergotamine, caffeine, and paracetamol in bulk and pharmaceutical formulation. The separation was carried out on silica gel plates, using ethyl acetate:ethanol:ammonia (9:1:0.1, v/v/v) as a developing system. Ultraviolet detection was carried out at 272 nm. The resulting retention times were 0.15, 0.36, 0.49, and 0.74 min for metoclopramide, ergotamine, caffeine, and paracetamol, respectively. The greenness profile assessment was achieved to the proposed method to evaluate its greenness characters to the environment with acceptable results. Validation parameters were checked according to International Conference of Harmonization guidelines to achieve the international requirements for quality control analysis of the proposed drugs.

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Dapoxetine hydrochloride (DAP) and Tadalafil (TAD) were separated and determined quantitatively using a validated green high-performance thin layer chromatographic (HPTLC) method in their binary mixtures either as raw materials or in pharmaceutical formulations. The concentration ranges were 0.1–1.6 and 0.2–2.5 μg/band for dapoxetine and tadalafil, respectively, with accuracies of 98.93% ± 0.62 and 99.26% ± 1.39, respectively. Silica gel HPTLC F254 plates were used to carry out the separation. The mobile phase used was a mixture of ethanol–ethyl acetate (1:9 by volume), which is environmentally green and harmless. Densitometric scanning with UV detector was used to detect the separated peaks at 222 nm. ICH guidelines were followed to validate the suggested method, and the results prove that they can be used for regular analysis in quality control laboratories with compatible results.

Background: Dapoxetine (DAP) is a serotonin-norepinephrine reuptake inhibitor, and Tadalafil (TAD) is a phosphodiesterase type-5 inhibitor. Both are coformulated as tablets called Erectafil® for treatment of erectile ejaculation. Objective: DAP and TAD were analyzed in their binary mixtures and pharmaceutical formulations using two multivariate calibration chemometric models. Methods: Partial least-squares (PLS) and linear support vector regression (SVR) models were applied using two factor-four level experimental design and UV-spectrophotometric data. They were compared to each other, and their advantages and disadvantages were discussed. Results: The developed methods succeeded to determine DAP and TAD in different ratios with good results regarding International Conference on Harmonization guidelines. Linearity ranges were 2–15 μg/mL and 3–30 μg/mL for DAP and TAD, respectively, with good accuracy of 100 ± 0.37 for DAP and 100 ± 0.8 for TAD regarding PLS model and 100.04 ± 0.32 for DAP and 99.89 ± 0.77 for TAD regarding SVR model. Good precision values of 0.787 for DAP and 0.793 for TAD regarding PLS model and 1.105 for DAP and 0.930 for TAD regarding SVR model were obtained. The two models were applied on the dosage forms and statistically compared with the published HPLC method with no significant difference regarding accuracy and precision. Conclusions: The two models can be utilized for routine analysis and QC of DAP and TAD in their bulk and pharmaceutical formulations. The SVR model gives better results and generalization ability than those of the PLS model regarding accuracy and prediction error, while the latter is better for being simpler and faster.

A validated RP-HPLC method was developed for the estimation of paracetamol, caffeine, metoclopramide and ergotamine simultaneously in bulk and pharmaceutical formulation. The method was extended for the determination of two paracetamol genotoxic and nephrotoxic impurities and degradation products namely p-aminophenol and 4-chloroacetanilide. Separation was done on octadecyl column (15 cm × 2.1 mm, 5 μm). Gradient elution was performed using mobile phase consisting of acetonitrile and water (pH 3) in ratio of (20: 80, v/v) for the first 3 min, (50: 50, v/v) for the next 4.5 min, then (20: 80, v/v) for the final 2.5 min. The flow rate was 0.7 mL/min throughout the run which took 10 min. UV detection was done at 230 nm. The proposed method agreed with ICH guidelines of method validation. The suggested method was applied for the estimation of the proposed drugs in their dosage form. Statistical comparison was done between the results obtained from the suggested method and those obtained from reported HPLC method. The proposed method is more beneficial than the published one because of having higher sensitivity and selectivity as it allows the detection of the proposed drugs in lower concentrations in the presence of paracetamol toxic impurities, p-aminophenol and 4-chloroacetanilide.