Coupling of Sequential Injection Chromatography with Multivariate Curve Resolution-Alternating Least-Squares for Enhancement of Peak Capacity

Abstract

Flow-through low-pressure chromatographic separations capitalized on the sequential injection chromatographic (SIC) concept are for the first time coupled to second-order multivariate regression models based on multivariate curve resolution-alternating least-squares (MCR-ALS) for outperforming current chromatographic methods in terms of resolution efficiency. The proposed SIC-MCR-ALS method involving sequential injection separation on short monolithic columns along with isocratic elution fosters ultrafast reversed-phase separations of complex multicomponent mixtures regardless of peak overlapping and retention parameters. The ruggedness of SIC systems is enhanced by removing the solenoid valves from the flow network, thus diminishing the column back pressure effects. As a consequence, the flow setup admitted mobile-phase flow rates much higher than those traditionally enabled in SIC. To ascertain the improved peak capacity of the SIC-MCR-ALS procedure, five phenolic species commonly used in disinfectant products and featuring similar UV spectra and close retention times in short reversed-phase silica-based monolithic phases are selected as model compounds and determined in just 1 min using mobile-phase flow rates of >or=2 mL min(-1). Notwithstanding the fact that the five phenolic derivatives coelute in a single chromatographic band, thus rendering resolution values ranging from 0.05 to 1.11, the concentration profiles and the pure spectra of each individual phenol species could be concurrently obtained. Quantitative validation of the chromatographic-chemometric method demonstrated both the reliability of the results and the enhanced resolution of mixtures with regard to former SIC systems with no need for thorough optimization of the separation conditions.