Determination of Chloroacetanilide Herbicide Metabolites in Water Using High-Performance Liquid Chromatography-Diode Array Detection and High-Performance Liquid Chromatography/Mass Spectrometry

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Abstract

Analytical methods using high-performance liquid chromatography-diode array detection (HPLC-DAD) and high-performance liquid chromatography/mass spectrometry (HPLC/MS) were developed for the analysis of the following chloroacetanilide herbicide metabolites in water: alachlor ethanesulfonic acid (ESA), alachlor oxanilic acid, acetochlor ESA, acetochlor oxanilic acid, metolachlor ESA, and metolachlor oxanilic acid. Good precision and accuracy were demonstrated for both the HPLC-DAD and HPLC/MS methods in reagent water, surface water, and ground water. The average HPLC-DAD recoveries of the chloroacetanilide herbicide metabolites from water samples spiked at 0.25, 0.5, and 2.0 mg/L (micrograms per liter) ranged from 84 to 112 percent, with relative standard deviations of 18 percent or less. The average HPLC/MS recoveries of the metabolites from water samples spiked at 0.05, 0.2, and 2.0 mg/L ranged from 81 to 118 percent, with relative standard deviations of 20 percent or less. The limit of quantitation (LOQ) for all metabolites using the HPLC-DAD method was 0.20 mg/L, whereas the LOQ using the HPLC/MS method was at 0.05 mg/L. These metabolite-determination methods are valuable for aquiring information about water quality and the fate and transport of the parent chloroacetanilide herbicides in water.

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Hostetler, K.A., and Thurman, E.M., 1999, Determination of chloroacetanilide herbicide metabolites in water using high-performance liquid chromatography-diode array detection and high-performance liquid chromatography/mass spectrometry, in Morganwalp, D.W., and Buxton, H.T., eds., U.S. Geological Survey Toxic Substances Hydrology Program--Proceedings of the technical meeting, Charleston, South Carolina, March 8-12, 1999, volume 2 of 3--Contamination of hydrologic systems and related ecosystems: U.S. Geological Survey Water-Resources Investigations Report 99-4018B, p. 345-353.

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