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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 27, Number 3, April 2003,
pp. 167-168
CASE REPORT: Determination of the Herbicide Glyphosate
and its Metabolite in Biological Specimens by Gas Chromatography–Mass
Spectrometry. A Case of Poisoning by Roundup® Herbicide
Yasushi Hori[1],[2], Manami Fujisawa[1],[2], Kenji
Shimada[1],
and Yasuo Hirose[3]
[1]Department of Analytical Chemistry, Faculty of Pharmaceutical Services, Niigata
University of Pharmacy and Applied Life
Sciences, Niigata, Japan;
[2]Department of Hospital pharmacy, Niigata City General
Hospital, Niigata, Japan; and
[3]Emergency and Critical Care Medical Center, Niigata City General Hospital,
Niigata,
Japan
In Japan, poisonings by the
glyphosate (GLYP)-containing herbicide Roundup and the gluphosinate (GLUF)-based
herbicide BASTA® have
been increasing since about 1987. We applied the gas chromatography–mass
spectrometry (GC–MS) method of analysis, on which we have already reported
in regard to the determination of the blood serum level of GLUF and its metabolite,
for the determination of serum and urinary levels of GLYP and its metabolite
aminomethyl phosphonic acid (AMPA). Derivatization using N-methyl-N-(tert-butyldimethylsilyl)
trifluoroacetamide was completed at a temperature of 80°C after 30 min,
and the detection limit of GLYP was 10 pg using m/z 454 and that of AMPA
was 1 pg using m/z 396. The full mass spectra of 100 pg GLYP and of 10 pg
AMPA were obtained easily. In extractions for which the Isolute® HAX
cartridge was employed, the mean recovery rate of GLYP and AMPA added to
serum to yield concentrations of 10–0.1 µg/mL (n = 5) was 91.6 ± 10.6%
(or better), whereas that of GLYP and AMPA added to urine to yield concentrations
of 100–1.0 µg/mL (n = 10) was 93.3 ± 6.6% (or better),
both of which were good rates. Also, using this method of analysis, the presence
of GLYP was identified in the full mass spectra obtained from the serum of
a patient who may or may not have ingested Roundup. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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