Milan Hutta, Róbert Góra
Comenius University in Bratislava, Faculty of Natural Sciences, Department of Analytical Chemistry, Ilkovičova 6, 84215 Bratislava, Slovakia
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Various natural substances are too complex analytes even for recent highly efficient analytical methods. One research approach is to characterize and analyze such complex systems is based on operational definition. Operationally defined analytes isolated from complex matrices resulted in development of novel combined multidimensional methods based on liquid chromatography separation with potential extension to combinations with electroseparation methods (ESM) and multi-detection (UV-VIS spectrophotometry, spectrofluorimetry, electroanalytical detection) and mass spectrometry (MS). Liquid chromatography working under extreme separation conditions (pH, ionic strength, temperature, additives, solvents etc.) as first dimension separation method is investigated. Usually, tough separation conditions are not directly compatible with the other methods in second separation dimension – some modes of HPLC, capillary isotachophoresis (ITP), capillary zone electrophoresis (CZE) (with various detection principles) and MS. Systematic study of orthogonality of novel combined techniques for characterization of operationally defined humic substances (HS) and/or lignin was done. Compatibility of used extreme extractive isolation and separation conditions in HPLC (ion exchange, reversed phase, size-exclusion) with common conditions of various end techniques was tested. The approach is valuable for solution of HS interferences elimination in soil samples containing pesticides. Comprehensive techniques of multidimensional liquid chromatography (under the conditions of extreme pH, I, temperature, large-volume injection, solid sample injection etc.) combined off-line or on-line with the other separation or identification methods are discussed. Application of methods combining extreme separation conditions in HPLC (pH within the range 0-2 or alternatively 10-14, ionic strength above 0.1 mol/l, temperature well above 40°C, non-common mobile phase solvents dimethylformamide) and normal separation conditions in ESM and MS in the field of environmental analysis, analysis of degradation products of soil humic substances.
The research was supported by the grant of projects APVV-17-0318, APVV-0462-20.
