SummaryThe potential of microcolumn liquid chromatography (FtLC) and capillary electrophoresis (CE) with on-line, flame photometric detection (FPD) in the P-selective mode has been studied for determination of polar P-containing pesticides, glyphosate and its main metabohte, aminomethylphosphonic acid (AMPA), ethephon, fosetyl-aluminium and acephate. Acephate was determined by reversed-phase ~LC-FPD using large-volume injections with peak compression, the other compounds were determined by ~LC-FPD and CE-FPD using simple, large-volume injection procedures to obtain limits of detection of 7.5-500 ng 9 mL 1. and 1.0 ~g 9 mL 1., respectively The methods showed acceptable repeatability and robustness and were successfully applied for rapid and selective determination of pesticides in fruit, vegetable and water samples.