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Methods of Analysis by the U.S. Geological Survey Organic Geochemistry Research Group—Determination of Glyphosate, Aminomethylphosphonic Acid, and Glufosinate in Water Using Online Solid-Phase Extraction and High-Performance Liquid Chromatography/Mass Spectrometry

Open-File Report 2001-454
By: , , and 
https://doi.org/10.3133/ofr01454

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Abstract

An analytical method for the determination of glyphosate, its principal degradation compound, aminomethylphosphonic acid (AMPA), and glufosinate in water with varying matrices has been developed. Four different sample matrices fortified at 0.2 and 2.0 μg/L (micrograms per liter) were analyzed using precolumn derivatization with 9-fluorenylmethylchloroformate (FMOC). After derivatization, cleanup and concentration were accomplished using automated online solid-phase extraction followed by elution with the mobile phase allowing for direct injection into a liquid chromatograph/mass spectrometer (LC/MS). Analytical conditions for MS detection were optimized, and quantitation was carried out using the following representative ions: 390 and 168 for glyphosate; 332, 110, and 136 for AMPA; and 402, 180, and 206 for glufosinate. Matrix effects were minimized by utilizing standard addition for quantification and an isotope-labeled glyphosate (2-13C,15N) as the internal standard. Method detection limits (MDLs) were 0.084 μg/L for glyphosate, 0.078 μg/L for AMPA, and 0.057 μg/L for glufosinate. The method reporting limits (MRLs) were set at 0.1 μg/L for all three compounds. The mean recovery values ranged from 88.0 to 128.7 percent, and relative standard deviation values ranged from 5.6 to 32.6 percent.

Suggested Citation

Lee, E. A., Strahan, A. P., and Thurman, E. M., 2001, Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group—Determination of glyphosate, aminomethylphosphonic acid, and glufonsinate in water using online solid-phase extraction and high-performance liquid chromatography/mass spectrometry: U.S. Geological Survey Open-File Report 01–454, 13 p., https://doi.org/10.3133/ofr01454.

ISSN: 2331-1258 (online)

Table of Contents

  • Abstract
  • Introduction
  • Determination of Glyphosate, Aminomethylphosphonic Acid, and Glufosinate in Water
  • Discussion
  • Conclusions
  • References Cited
  • Appendices
Publication type Report
Publication Subtype USGS Numbered Series
Title Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group—Determination of glyphosate, aminomethylphosphonic acid, and glufonsinate in water using online solid-phase extraction and high-performance liquid chromatography/mass spectrometry
Series title Open-File Report
Series number 2001-454
DOI 10.3133/ofr01454
Year Published 2001
Language English
Publisher U.S. Geological Survey
Publisher location Reston, VA
Contributing office(s) Kansas Water Science Center, Toxic Substances Hydrology Program
Description iv, 13 p.
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