Gas chromatographic simultaneous determination of organophosphorus pesticides in feed after clean-up by gel-permeation chromatography and solid-phase extraction

• Published in: BUNSEKI KAGAKU Vol. 46; no. 2; pp. 121 - 130
• Main Authors: HIBINO, Hiroshi, SUZUKI, Shigetaka, HAYAKAWA, Toshiaki, SHIRAI, Yuji
• Format: Journal Article
• Language: English; Japanese
• Published: Tokyo The Japan Society for Analytical Chemistry 01.01.1997; Japan Science and Technology Agency
• Subjects: capillary gas chromatography (GC); charcoal activate cartridge; Florisil cartridge; gel permeation chromatography (GPC); organophosphorus pesticide
• ISSN: 0525-1931
• DOI: 10.2116/bunsekikagaku.46.121

An analytical method for organophosphorus pesticides in feed was established by capillary column gas chromatography. After water was added to a sample, the pesticides were simultaneously extracted with acetonitrile. The extract was purified with a gelpermeation chromatograph on a stainless-steel column (20 mm i.d. X 300 mm), followed with a Florisil cartridge or a charcoal activate cartridge. The pesticides were simultaneously determined by a gas chromatograph equipped with a FPD on a fussed silica capillary column bonded 5% diphenyl 95% dimethyl polysiloxane or trifluoropropylmethyl polysiloxane (0.25 mm i.d. × 300 mm, 0.25 μm film tiness). The recovery test was conducted with mixed feed and hay (alfalfa) spiked with pesticides at levels of 0.022.0 ppm. Except for metamidophos and tiometon, the mean recoveries at levels of more than 0.02 ppm were in the range of 73119%, and the relative standard deviation of repeatability (RSDr) was within 14%. A cross check test was carried out at 3 laboratories with mixed feed spiked with the pesticides at levels of 1.0 ppm. The mean recoveries were in the range of 80129%, and the relative standard deviation of reproducibility (RSDR) was within 20%.