A simple reliable quantification of glyphosate in human urine using MonoSpin TiO extraction and isotope dilution mass spectrometry

Takamitsu Otake; Keisuke Nakamura; Nobuyasu Hanari

doi:10.1584/jpestics.D23-030

A simple reliable quantification of glyphosate in human urine using MonoSpin TiO extraction and isotope dilution mass spectrometry

J Pestic Sci. 2023 Nov 20;48(4):137-148. doi: 10.1584/jpestics.D23-030.

Authors

Takamitsu Otake¹, Keisuke Nakamura¹, Nobuyasu Hanari¹

Affiliation

¹ National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology.

Abstract

A method of quantifying glyphosate (Gly) in human urine by means of MonoSpin TiO extraction and 9-fluorenylmethoxycarbonyl chloride (FMOC-Cl) derivatization with isotope dilution mass spectrometry (IDMS) was investigated and optimized. The method's quantification limit under optimized conditions was 0.3 µg/kg for FMOC-Gly, which was comparable to or lower than those described in previous studies. When a spike test using human urine samples was carried out with optimized analytical conditions, the trueness for FMOC-Gly was as follows: 101.6-104.9% for a spike level of 0.5 µg/kg and 99.2-101.0% for a spike level of 30 µg/kg. The intra-day repeatability and inter-day reproducibility were <6.5%. The spike test results for validation between the "with" and "without" derivatization methods were comparable at 1 µg/kg. Our results indicate that using MonoSpin TiO extraction and FMOC-Cl derivatization with IDMS is an accurate method for analyzing Gly in human urine.

Keywords: FMOC-Cl derivatization; MonoSpin TiO extraction; glyphosate; human urine; isotope dilution mass spectrometry (IDMS).