Ultra-trace Analysis of Metosulam,a New Triazolopyrimidine Herbicide,in Soil Using LC-UV and TSP-LC-MS

Abstract

Metosulam (DE-511), N-(2,6-dichloro-m-tolyl)-5,7-dimethoxy-[1,2,4] triazolo [1,5a]pynmidine-2-sulphonamide is a new selective herbicide developed for the control of broadleaf weeds in cereals and maize.

The application of new generation low use rate herbicides, such as metosulam, has in turn created the need for the development of ultra-trace residue methodologies. To help investigate the environmental impact of metosulam, levels at sub-part per billion (μg/kg) in soil were determined.

Application of capillary gas chromatography, with various injector systems, was unable to analyse metosulam methyl derivative due to the inherent thermal instability of the molecule. Liquid chromatography with ultraviolet detection (LC-UV) was used to quantify residues of the herbicide following a series of selective clean-up procedures. The chosen methodology used simple reagents plus standard equipment and although the molar absorbtivity of metosulam is poor, analysis of soils of various texture classes at the desired sensitivity level, was achieved.

Thermospray Liquid chromatography with mass spectrometry (TSP-LC-MS) was used as a confirmatory technique for the analysis of metosulam in the same soils. Excellent agreement between the two techniques was observed.

Details of the clean-up procedures used to produce desired selectivity and the relative merit of the two detection systems are discussed.