Metallofluorescent indicators as spray reagents for the in situ determination of organophosphorus pesticides on thin-layer chromatograms

Abstract

Fluorescence-quenched solutions of palladium(II)-calcein and palladium(II)-calcein blue are shown to be sensitive spray reagents for the detection and in situ determination of organothiophosphorus insecticides on thin-layer chromatograms. The palladium is displaced from its non-fluorescent indicator complex by the pesticide producing fluorescent spots on the plate. Visual detection limits for 16 insecticides are given. As little as 10–50 ng of phosphorodithioate pesticides can be detected within l h after spraying and drying the plate, while the detection limits for phosphorothioates are somewhat higher ( ca. 50–100 ng). Quantitative measurements may be conveniently made 18–24 h after spraying and drying the plate. Plots of fluorescence (as peak area) versus quantity of pesticide are linear over a 10–15 fold range. The relative standard deviation of replicate spots of Guthion (50–400 ng) and Cygon (50–100 ng) is 4–9 % and less than 15 % for 10 ng of Cygon or 20 ng of Guthion. The method was applied to the analysis of lake water spiked with Cygon. The recovery of 2–20 μg l -1 of the pesticide was 87–113% with no clean-up other than t.l.c. required.