title: Quantitation of neonicotinoid metabolites in human urine using GC-MS.
abstract: A rapid and sensitive analytical method using gas chromatography-mass spectrometry (GC-MS) was developed for the measurement of neonicotinoid (NEO) metabolites 6-chloronicotinic acid (6CN), 2-chloro-1,3-thiazole-5-carboxylic acid (2CTCA) and 3-furoic acid (3FA) from human urine. After acid hydrolysis, the metabolites were extracted using solid phase extraction (SPE) column (Bond Elute Plexa PCX) and eluted with methanol. N,O-bis (trimethylsilyl) trifluoroacetamide with 1% trimethylchlorosilane (BSTFA-TMCS, 99:1) was used for the derivatization of metabolites and analyzed by GC-MS with the electron ionization mode. The elution solvent, derivatization reagent and its conditions were mainly optimized for improved detection and quantitation of the metabolites based on signal-to-noise ratio, recoveries and reproducibility. Our present method offered a sufficiently low limit of detection (0.1μg/L for each metabolite) with satisfactory within-run and between-day accuracy and precision (variability less than 12.3%, R.S.D). This method is simple, sensitive and precise, and has been successfully applied to quantify low concentrations of urinary 6CN, 2CTCA and 3FA for the occupational NEO exposures survey.
authors.affiliation: Department of Pathophysiological Laboratory Sciences, Field of Radiological and Medical Laboratory Sciences, Nagoya University Graduate, School of Medicine, Nagoya 461-8673, Japan.
authors.forename: Hiroshi
authors.initials: H
authors.lastname: Nomura
authors.forename: Jun
authors.initials: J
authors.lastname: Ueyama
authors.forename: Takaaki
authors.initials: T
authors.lastname: Kondo
authors.forename: Isao
authors.initials: I
authors.lastname: Saito
authors.forename: Katsuyuki
authors.initials: K
authors.lastname: Murata
authors.forename: Toyoto
authors.initials: T
authors.lastname: Iwata
authors.forename: Shinya
authors.initials: S
authors.lastname: Wakusawa
authors.forename: Michihiro
authors.initials: M
authors.lastname: Kamijima
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D007306:Insecticides / Q000652:urine*; D057230:Limit of Detection; D009538:Nicotine / Q000652:urine*; D012015:Reference Standards; D015203:Reproducibility of Results
chemical_list: D007306:Insecticides; D009538:Nicotine
keywords: GC-MS; Metabolite; Neonicotinoid; Urine