Sensitive determination of methomyl in blood using gas chromatography-mass spectrometry as its oxime tert.-butyldimethylsilyl derivative

Shinji Ito, Keiko Kudo, Tohru Imamura, Tsuneo Suzuki, Noriaki Ikeda

Research output: Contribution to journalArticle

13 Citations (Scopus)

Abstract

A sensitive, selective and reliable method was developed to determine methomyl {methyl-N-[(methylcarbamoyl)oxy]thioacetimidate}, a carbamate insecticide in human blood, using gas chromatography-mass spectrometry. Dimethylglyoxime served as an internal standard (I.S.). Methomyl in the blood was converted to its oxime form by sodium hydroxide. The solution made acidic with hydrochloric acid was poured into a column packed with Extrelut. Methomyloxime and I.S. were eluted from the column with a mixture of dichloromethane-ethyl acetate-chloroform (65:25:10), transformed to tert.-butyldimethylsilyl derivatives, and analyzed by gas chromatography-mass spectrometry in the electron impact mode. The calibration curves were linear in the concentration range from 1 ng/g to 100 ng/g and 100 ng/g to at least 5000 ng/g. The lower limit of detection was 0.5 ng/g. The absolute recoveries were 72-93% and within-day coefficients of variation were 3.1-5.6% at blood concentrations of 10 and 1000 ng/g. Two practical forensic applications are described. Copyright (C) 1998 Elsevier Science B.V.

Original languageEnglish
Pages (from-to)323-330
Number of pages8
JournalJournal of Chromatography B: Biomedical Applications
Volume713
Issue number2
DOIs
Publication statusPublished - Aug 25 1998

All Science Journal Classification (ASJC) codes

  • Chemistry(all)

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