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A novel chemometric strategy was implemented in the development of a new ultraperformance liquid chromatography method for the quantitative estimation of guaifenesin and pseudoephedrine hydrochloride in a two-component syrup formulation with minimal experimental effort, time and reagent. A full factorial design with three factors was investigated to find optimal working conditions of chromatographic factors (column temperature, flow rate, and 0.1 M H3PO4% in mobile phase) that affect the chromatographic separation. Then, optimum experimental conditions providing adequate separation of the analyzed drug substances within the short runtime were determined. Under optimal experimental conditions, the retention times for guaifenesin and pseudoephedrine hydrochloride were obtained as 0.817 and 1.430 min, respectively. In the optimized RP-UPLC method, chromatographic response was reported as a linear function of concentration between 5.0 and 80.0 μg/mL for guaifenesin and 10.0–90.0 μg/mL for pseudoephedrine hydrochloride. The proposed method was carefully validated and successfully applied to quality control and analysis of a cough syrup preparation containing guaifenesin and pseudoephedrine hydrochloride. Consequently, the proposed reversed-phase ultraperformance liquid chromatography method provided an opportunity to quantify relevant drugs with small amount of reagents and short runtime. [ABSTRACT FROM AUTHOR]

Poor chromatographic resolution is one of the main challenges in chromatographic analysis. Partially separated chromatographic peaks frequently occur, due to the nature of analytes and the demand for fast analysis using high flow rates and shorter columns. Modeling of chromatographic three‐way data using suitable chemometric tools enables determining co‐eluted peaks without using additional experimental efforts. In this paper, parallel factor analysis (PARAFAC) was applied to chromatographic data for the quantitative resolution of a quaternary mixture at the co‐elution condition of acetaminophen, aspirin, ascorbic acid, and guaifenesin in a spectrochromatogram. The spectrochromatograms of the calibration set, validation set, and real samples were arranged as a three‐way array. In the next step, the PARAFAC model was implemented to decompose the spectrochromatographic array into trilinear components, corresponding to spectral, chromatographic, and relative concentration profiles of the analytes. The chromatographic and spectral modes were used for the qualitative analysis of components, whereas the analytes in commercial tablets were quantified from their individual profiles in their concentration mode. This study indicated that the application of the PARAFAC model provided a novel strategy for determining overlapping peaks in a chromatogram to perform the analysis of multicomponent mixtures with reduced runtime and without additional efforts. [ABSTRACT FROM AUTHOR]

This paper presents a new application of three-way parallel factor analysis (3W-PARAFAC) model to the coeluting spectrochromatograms for the quantitative resolution of a quaternary mixture system consisting of paracetamol, propyphenazone, and caffeine with aspirin as an internal standard. Spectrochromatograms of calibration standards, validation sets, and unknown samples were recorded as a function of retention time and wavelength in the range of 0.0–2.5 min and 200–400 nm, respectively, using ultra-performance liquid chromatography with photodiode array detection (UPLC-PDA). Three-way UPLC-PDA data arrayX(retention time × wavelength × sample) was obtained from the data matrices of the spectrochromatograms. 3W-PARAFAC decomposition of three-way UPLC-PDA data array provided three loading matrices corresponding to chromatographic mode, spectral mode, and relative concentration mode. Quantitative estimation of paracetamol, propyphenazone, and caffeine in analyzed samples was accomplished using the relative concentration mode obtained by the deconvolution of the UPLC-PDA data set. The validity and ability of 3W-PARAFAC model were checked by analyzing independent test samples. It was observed from analyses that 3W-PARAFAC method has potential to uniquely resolve strongly overlapping peaks of analyzed compounds in a spectrochromatogram, which was obtained under experimental conditions consisting of the lower flow rate, short run time, and simple mobile phase composition. The proposed three-way chemometric approach was successfully applied to the simultaneous quantification of paracetamol, propyphenazone, and caffeine in tablets. Experiments showed that the determination results were in good agreement with label amount in commercial pharmaceutical preparation. [ABSTRACT FROM PUBLISHER]

Introduction: Co-elution is a common challenge in phytochemical chromatography. Full chromatographic separation often requires extensive optimization, long analysis times, and excessive solvent use. A viable alternative could be mathematical elution of analytes using three-dimensional decomposition., Objectives: This study aimed to develop a method to determine chlorogenic acid in Melampyrum stenophyllum Boiss. extracts without complete chromatographic separation, to validate the method, and to cross-validate assay results against a classical ultra-performance liquid chromatography (UPLC) method., Methodology: Ultra-performance liquid chromatography-photodiode array (UPLC-PDA) spectrochromatograms were arranged into a three-way data cube with dimensions of time, wavelength, and sample and then decomposed using parallel factor analysis to reveal chromatographic, spectral, and concentration profiles. The chromatographic and spectral profiles were used to identify chlorogenic acid in overlapping signals. The relative concentration profile was used to quantify it in the plant extract. The assay results were statistically compared with those from an in-house classical UPLC method., Results: Chlorogenic acid was co-eluted at 1.45 min and quantified as 16.11 mg per gram dry weight of Melampyrum stenophyllum extracts (SD = 0.28), despite significant interference in a 4-min runtime. The analytical validity was confirmed by recovery calculations from standard solutions and standard addition samples (RSD < 2%), and the t-test resulted in a p-value of 0.09 (α = 0.05), indicating no significant difference between the results obtained from mathematical elution and chromatographic separation., Conclusion: Chlorogenic acid was quantified from plant material accurately despite the co-elution. Validation and cross-validation results support the method's applicability., (© 2024 The Author(s). Phytochemical Analysis published by John Wiley & Sons Ltd.)