Automated continuous-flow in-syringe dispersive liquid-liquid microextraction of mono-nitrophenols from large sample volumes using a novel approach to multivariate spectral analysis

K Fikarová; B Horstkotte; H Sklenářová; F Švec; P Solich

doi:10.1016/j.talanta.2019.04.044

Automated continuous-flow in-syringe dispersive liquid-liquid microextraction of mono-nitrophenols from large sample volumes using a novel approach to multivariate spectral analysis

Talanta. 2019 Sep 1:202:11-20. doi: 10.1016/j.talanta.2019.04.044. Epub 2019 Apr 21.

Authors

K Fikarová¹, B Horstkotte², H Sklenářová¹, F Švec¹, P Solich¹

Affiliations

¹ Charles University, Faculty of Pharmacy in Hradec Králové, Department of Analytical Chemistry, Akademika Heyrovského 1203, 500 05, Hradec Králové, Czech Republic.
² Charles University, Faculty of Pharmacy in Hradec Králové, Department of Analytical Chemistry, Akademika Heyrovského 1203, 500 05, Hradec Králové, Czech Republic. Electronic address: Horstkob@faf.cuni.cz.

PMID: 31171158
DOI: 10.1016/j.talanta.2019.04.044

Abstract

Continuous magnetic stirring-assisted dispersive liquid-liquid extraction followed by dispersive backextraction as a novel pre-treatment technique for adaptable and milliliter volumes of environmental samples has been developed. The procedure was automated using the technique "Lab-In-Syringe". The void of the automated syringe pump was used as size-adaptable extraction chamber. By a flow channel in the syringe piston, continuous flow through the syringe void was enabled. 1-Octanol was used as an extractant and dispersed by the action of a magnetic stirring bar, which was placed inside the syringe and driven by an external rotating magnetic field. Extract washing and dispersive backextraction in an alkaline aqueous acceptor phase were carried out after the preceding extraction from the acidified water sample. Analyte determination was achieved using multivariate spectrum analysis. The method was applied to determine priority pollutants, mono-nitrophenols, in surface water and enabled to reach limits of detection for o-, m-, p-nitrophenol (λ = 418, 390, 400 nm, respectively) of 0.14, 0.26, and 0.02 μmol L^-1 (19.5, 36.2, and 2.8 μg L^-1), respectively. Under optimized conditions, relative standard deviations were generally less than 5% and enrichment factors of o-, m-, p-nitrophenol 19, 25, and 21, respectively, were achieved using sample volumes of up to 24 mL. Average recoveries of o-, m-, p-nitrophenol from spiked surface water were 94, 82, and 92%, respectively. The concentration of humic acid was found 6-times reduced with respect to the analyte. In addition, adding spectral background modeling allowed nitrophenol determination with precision adequate for routine analysis.

Keywords: Background simulation; Continuous-flow dispersive liquid-liquid microextraction; Lab-in-Syringe; Large volume sample pre-treatment; Mono-nitrophenols; Multivariate spectrum analysis.