Headspace gas chromatography of stimulants in urine by in-column trifluoroacetyl derivatization method.
The analysis of stimulants in urine using a headspace gas chromatography system equipped with an in-column sample trifluoroacetylation unit was investigated. A 5-ml aliquot of urine containing stimulants was pipetted into a 20-ml autosampler vial together with 3.5 g of potassium carbonate. The vial was sealed and heated for 20 min at 80 degrees C, then 0.8 ml of the headspace gas and N-methylbis(trifluoroacetamide) gas were injected simultaneously into the gas chromatograph equipped with a flame ionization detector and a fused-silica capillary column (DB-1, 30 m x 0.32 mm I.D., film thickness 0.25 micron), with a gas-tight syringe. Calibration graphs prepared by the absolute calibration curve method showed good linearity over the concentration range of 0.04 to 50 micrograms/ml for methamphetamine hydrochloride and amphetamine sulphate. The detection limits were 0.03 micrograms/ml for both of these compounds.
Tsuchihashi
H
H
Forensic Science Laboratory, Osaka Prefectural Police Head Quarters, Japan.
Nakajima
K
K
Nishikawa
M
M
Shiomi
K
K
Takahashi
S
S
D000081:Acetamides; D000661:Amphetamine / Q000652:urine*; D002849:Chromatography, Gas; D005463:Fluoroacetates; D006801:Humans; D007202:Indicators and Reagents; D008694:Methamphetamine / Q000652:urine*; D013696:Temperature
D000081:Acetamides; D005463:Fluoroacetates; D007202:Indicators and Reagents; D008694:Methamphetamine; C014666:N-methyl-bis(trifluoroacetamide); D000661:Amphetamine