High-pressure liquid chromatography of neurotoxic phenylphosphonothioate esters and related compounds.
Lasker-JM; Sivarajah-K; Eling-TE; Abou-Donia-MB
Anal Biochem 1980 Dec; 109(2):369-375
A chromatographic method for determining neurotoxic phenylphosphonothioate esters was developed. Five to 25 microliter samples containing leptophos (21609905), O-2,5-dichlorophenyl-O- methyl-phenylphosphonothioate (53490781) (desbromoleptophos), O- ethyl-O-4-nitrophenylphenylphosphonothioate (2104645) (EPN), cyanofenphos (13067931), and O-ethyl-O-2,4-dichlorophenyl- phenylphosphonothioate (3792594) (EPBP) were injected into a reversed phase high pressure liquid chromatography system containing a microparticulate RP-8 column and an ultraviolet detector operating at 280 nanometers. The mobile phase was varied from 1% methanol, 5% glacial-acetic-acid and 95% water to 95% methanol and 5% water over 30 minutes using a gradient elution technique following a 10 minute isocratic delay. Leptophos, desbromoleptophos, EPN, cyanofenphos, and EPBP were well separated from each other and from their degradation products, which included oxygen analogues and phenols. The detection limit for EPN was 0.01 microgram (microg). The detection limit for leptophos, cyanofenphos, desbromoleptophos, and EPBP was 0.1microg. The relationship between the detector response (peak area) and amounts injected was linear over at least a 100 fold range. The technique was applied to determining the metabolites formed when EPN was incubated with rat liver microsomes in the presence of NADPH. The authors conclude that the technique can rapidly determine leptophos, desbromoleptophos, EPN, cyanofenphos, and EPBP. Only a single chromatographic step is required to perform the analysis.
NIOSH-Publication; NIOSH-Grant; Neurotoxic-effects; Analytical-methods; Organo-phosphorus-pesticides; Chromatographic-analysis; Biotransformation; Liver-microsomes
Pharmacology Duke University Department of Pharmacology Durham, N C 27710
21609-90-5; 53490-78-1; 2104-64-5; 13067-93-1; 3792-59-4
Neurotoxic Disorders; Neurotoxic-effects
Duke University, Durham, North Carolina