title: Automated procedure for determination of barbiturates in serum using the combined system of PrepStation and gas chromatography-mass spectrometry.
abstract: A system of an automatic sample preparation procedure followed by on-line injection of the sample extract into a gas chromatograph-mass spectrometer (GC-MS) was developed for the simultaneous analysis of seven barbiturates in human serum. A 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 1.5 ml of a diluted serum 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 the GC-MS. The calibration curves, using an internal standard method, demonstrated a good linearity throughout the concentration range from 0.1 to 10 microg ml(-1) for all barbiturates extracted. The proposed method was applied to 27 clinical serum samples from three patients who were administrated secobarbital.
authors.affiliation: Department of Legal Medicine, Hiroshima University School of Medicine, Japan.
authors.forename: A
authors.initials: A
authors.lastname: Namera
authors.forename: M
authors.initials: M
authors.lastname: Yashiki
authors.forename: Y
authors.initials: Y
authors.lastname: Iwasaki
authors.forename: M
authors.initials: M
authors.lastname: Ohtani
authors.forename: T
authors.initials: T
authors.lastname: Kojima
mesh_terms: D000328:Adult; D001322:Autoanalysis; D001463:Barbiturates / Q000097:blood*; D001798:Blood Proteins; D002021:Buffers; D011232:Chemical Precipitation; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D008297:Male; D000432:Methanol; D010710:Phosphates; D011786:Quality Control; D012631:Secobarbital / Q000008:administration & dosage / Q000097:blood; D014867:Water
chemical_list: D001463:Barbiturates; D001798:Blood Proteins; D002021:Buffers; D010710:Phosphates; D014867:Water; D012631:Secobarbital; D000432:Methanol