TY - JOUR
T1 - Sensitive determination of methomyl in blood using gas chromatography-mass spectrometry as its oxime tert.-butyldimethylsilyl derivative
AU - Ito, Shinji
AU - Kudo, Keiko
AU - Imamura, Tohru
AU - Suzuki, Tsuneo
AU - Ikeda, Noriaki
PY - 1998/8/25
Y1 - 1998/8/25
N2 - 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.
AB - 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.
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U2 - 10.1016/S0378-4347(98)00198-4
DO - 10.1016/S0378-4347(98)00198-4
M3 - Article
C2 - 9746247
AN - SCOPUS:0032443382
VL - 713
SP - 323
EP - 330
JO - Journal of Chromatography B: Biomedical Sciences and Applications
JF - Journal of Chromatography B: Biomedical Sciences and Applications
SN - 0378-4347
IS - 2
ER -