Sensitive determination of methomyl in blood using gas chromatography-mass spectrometry as its oxime tert.-butyldimethylsilyl derivative.
J Chromatogr B Biomed Sci Appl
; 713(2): 323-30, 1998 Aug 25.
Article
en En
| MEDLINE
| ID: mdl-9746247
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 (652510), 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.
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Colección:
01-internacional
Base de datos:
MEDLINE
Asunto principal:
Compuestos de Organosilicio
/
Fluoroacetatos
/
Insecticidas
/
Metomil
Tipo de estudio:
Diagnostic_studies
Límite:
Adult
/
Female
/
Humans
/
Male
/
Middle aged
Idioma:
En
Revista:
J Chromatogr B Biomed Sci Appl
Asunto de la revista:
QUIMICA CLINICA
Año:
1998
Tipo del documento:
Article
País de afiliación:
Japón