title: Rapid determination of glyphosate, glufosinate, bialaphos, and their major metabolites in serum by liquid chromatography-tandem mass spectrometry using hydrophilic interaction chromatography.
abstract: We developed a simple and rapid method for the simultaneous determination of phosphorus-containing amino acid herbicides (glyphosate, glufosinate, bialaphos) and their major metabolites, aminomethylphosphonic acid (AMPA) and 3-methylphosphinicopropionic acid (MPPA), in human serum. Serum samples were filtrated through an ultrafiltration membrane to remove proteins. The filtrate was then washed with chloroform, and injected into a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. Chromatographic separation was achieved on a hydrophilic interaction chromatography (HILIC) column. Determination of the target herbicides and metabolites was successfully carried out without derivatization or solid phase extraction (SPE) cartridge clean-up. The recoveries of these compounds, added to human serum at 0.2μg/mL, ranged from 94% to 108%, and the relative standard deviations (RSDs) were within 5.9%. The limits of detection (LODs) were 0.01μg/mL for MPPA, 0.02μg/mL for AMPA, 0.03μg/mL for both glyphosate and glufosinate, and 0.07μg/mL for bialaphos, respectively.
authors.affiliation: Hyogo Prefectural Institute of Public Health and Consumer Sciences, 2-1-29, Arata-cho, Hyogo-ku, Kobe 652-0032, Japan. Naoki Yoshioka@pref.hyogo.lg.jp
authors.forename: Naoki
authors.initials: N
authors.lastname: Yoshioka
authors.forename: Migiwa
authors.initials: M
authors.lastname: Asano
authors.forename: Azumi
authors.initials: A
authors.lastname: Kuse
authors.forename: Takao
authors.initials: T
authors.lastname: Mitsuhashi
authors.forename: Yasushi
authors.initials: Y
authors.lastname: Nagasaki
authors.forename: Yasuhiro
authors.initials: Y
authors.lastname: Ueno
mesh_terms: D000613:Aminobutyrates / Q000097:blood; D002853:Chromatography, Liquid / Q000379:methods*; D005260:Female; D005554:Forensic Medicine; D005998:Glycine / Q000031:analogs & derivatives / Q000097:blood; D006540:Herbicides / Q000097:blood*; D006801:Humans; D057927:Hydrophobic and Hydrophilic Interactions; D007555:Isoxazoles; D008297:Male; D008875:Middle Aged; D063065:Organophosphonates / Q000097:blood; D009943:Organophosphorus Compounds / Q000097:blood; D011422:Propionates / Q000097:blood; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013777:Tetrazoles; D000097797:Glyphosate
chemical_list: D000613:Aminobutyrates; D005998:Glycine; D006540:Herbicides; D007555:Isoxazoles; D063065:Organophosphonates; D009943:Organophosphorus Compounds; D011422:Propionates; D013777:Tetrazoles; D000097797:Glyphosate; C417734:AE F061517; C003122:bialaphos; C003121:phosphinothricin; C418233:2-amino-3-(3-hydrox-5(2-methyl-2H-tetrazol-5-yl)isoxazol-4-yl)propionic acid