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

研究成果: Contribution to journalArticle査読

13 被引用数 (Scopus)

抄録

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.

本文言語英語
ページ(範囲)323-330
ページ数8
ジャーナルJournal of Chromatography B: Biomedical Applications
713
2
DOI
出版ステータス出版済み - 8 25 1998

All Science Journal Classification (ASJC) codes

  • 化学 (全般)

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