Determination of glufosinate ammonium and its metabolite, 3-methylphosphinicopropionic acid, in human serum by gas chromatography-mass spectrometry following mixed-mode solid-phase extraction and t-BDMS derivatization.
A method for the analysis of glufosinate ammonium (GLUF) and its metabolite 3-methylphosphinicopropionic acid (MPPA) in human serum by gas chromatography-mass spectrometry (GC-MS) was developed. Employing a mixed-mode cartridge with both anion exchange action and weak nonpolar interaction, we extracted GLUF and MPPA from the serum and carried out GC-MS analysis of their tert-butyldimethylsilyl derivatives. The detection limits of GLUF and MPPA were 10 pg and 1 pg, respectively. Full mass spectra of 100 pg GLUF and of 10 pg MPPA were easily obtainable. The recovery rate of 90.0+/-11.9% (or better) when the serum concentrations of GLUF and MPPA were 10-0.1 microg/mL. Results of 23 serum samples, from patients with GLUF poisoning, measured by this method correlate well with those derived from the conventional high-performance liquid chromatography method (r = 0.996). The developed GC-MS method is likely to become a useful analytical technique in clinical settings.
Hori
Y
Y
Department of Analytical Chemistry, Niigata College of Pharmacy, Japan. horiy@med.niigata-u.ac.jp
Fujisawa
M
M
Shimada
K
K
Hirose
Y
Y
D000613:Aminobutyrates / Q000097:blood* / Q000737:chemistry / Q000506:poisoning; D002623:Chemistry Techniques, Analytical / Q000379:methods; D002851:Chromatography, High Pressure Liquid; D008401:Gas Chromatography-Mass Spectrometry; D006540:Herbicides / Q000097:blood* / Q000737:chemistry / Q000506:poisoning; D006801:Humans; D062025:Organophosphate Poisoning; D063065:Organophosphonates / Q000097:blood* / Q000737:chemistry; D011041:Poisoning / Q000175:diagnosis; D011422:Propionates / Q000097:blood* / Q000737:chemistry / Q000506:poisoning; D012680:Sensitivity and Specificity
C417734:AE F061517; D000613:Aminobutyrates; D006540:Herbicides; D063065:Organophosphonates; D011422:Propionates; C003121:phosphinothricin