Automated preparation and analysis of barbiturates in human urine using the combined system of PrepStation and gas chromatography-mass spectrometry.
A system for an automatic sample preparation procedure followed by on-line injection of the sample extract into a gas chromatography-mass spectrometry (GC-MS) system was developed for the simultaneous analysis of seven barbiturates in human urine. Sample clean-up was performed by a solid-phase extraction (SPE) on a C18 disposable cartridge. A SPE cartridge was preconditioned with methanol and 0.1 M phosphate buffer. After loading a 1.5 ml volume of a urine sample into the SPE cartridge, the cartridge was washed with 2.5 ml of methanol-water (1:9, v/v). Barbiturates were eluted with 1.0 ml of chloroform-isopropanol (3:1, v/v) from the cartridge. The eluate (1 microl) was injected into a GC-MS system. The calibration curves, using an internal standard method, demonstrated a good linearity throughout the concentration range from 0.02 to 10 microg/ml for all barbiturates extracted. The proposed method was applied to several clinical cases. The total analysis time for 20 samples was approximately 14 h.
Namera
A
A
Department of Legal Medicine, Hiroshima University School of Medicine, Japan.
Yashiki
M
M
Okada
K
K
Iwasaki
Y
Y
Ohtani
M
M
Kojima
T
T
D000328:Adult; D001463:Barbiturates / Q000145:classification / Q000652:urine*; D002940:Circadian Rhythm; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D006863:Hydrogen-Ion Concentration; D006993:Hypnotics and Sedatives / Q000145:classification / Q000652:urine*; D016014:Linear Models; D008297:Male; D008875:Middle Aged; D009862:Online Systems; D015203:Reproducibility of Results
D001463:Barbiturates; D006993:Hypnotics and Sedatives