Determination by glyphosate and aminomethylphosphonic acid in crops by capillary gas chromatography with mass-selective detection: collaborative study

J AOAC Int. 2001 May-Jun;84(3):823-46.

Abstract

A collaborative study was conducted to validate a method for the determination of glyphosate and aminomethylphosphonic acid (AMPA) in crops. The analytes are extracted from crops with water, and the crude extracts are then subjected to a cation exchange cleanup. The analytes are derivatized by the direct addition of the aqueous extract into a mixture of heptafluorobutanol and trifluoroacetic anhydride. The derivatized analytes are quantitated by capillary gas chromatography with mass-selective detection (MSD). The collaborative study involved 13 laboratories located in 5 countries; 12 laboratories returned valid data sets. The crops tested were field corn grain, soya forage, and walnut nutmeat at concentrations of 0.050, 0.40, and 2.0 mg/kg. The study used a split-level pair replication scheme with blindly coded laboratory samples. Twelve materials were analyzed, including 1 control and 3 split-level pairs for each matrix, 1 pair at each nominal concentration. For glyphosate, the mean recovery was 91%, the average intralaboratory variance, the repeatability relative standard deviation (RSDr), was 11%, and the interlaboratory variance, the reproducibility relative standard deviation (RSDR), was 16%. For AMPA, the mean recovery was 87%, the RSDr was 16%, and the RSDR was 25% at mg/kg levels.

Publication types

  • Validation Study

MeSH terms

  • Chromatography, Gas / methods*
  • Crops, Agricultural / chemistry*
  • Glycine / analogs & derivatives*
  • Glycine / analysis*
  • Glycine max / chemistry
  • Glyphosate
  • Herbicides / analysis*
  • Laboratories / standards
  • Nuts / chemistry
  • Organophosphorus Compounds / analysis*
  • Quality Control
  • Reproducibility of Results
  • Zea mays / chemistry

Substances

  • Herbicides
  • Organophosphorus Compounds
  • 1-aminomethylphosphonic acid
  • Glycine