A rapid method for detecting barbiturates in serum using EI-SIM.
A simple and rapid method for analysis of barbiturates in serum has been developed. In order to extract and clean barbiturates in serum, a separation column packed with Extrelut and Florisil was used, and the eluate was directly analyzed by means of electron impact selected ion monitoring (EI-SIM). Selected ions used were base peak ions of 10 barbituartes, and the internal standard used was allobarbital or secobarbital. The calibration curves were linear over the range 0.5-5 ng. Extraction of replicate serum samples containing 20 micrograms/1.5 ml and 5 micrograms/1.5 ml resulted in a recovery of 87.2-105.2% and 81.6-104.6%, respectively, with the exception of phenobarbital, which was 151.9% and 172.1%, respectively. Secobarbital was also analyzed in the serum of 13 patients who had been given secobarbital intravenously. In 3 out of 10 cases, secobarbital levels greater than 1 micrograms/ml were detected more than 72 h after administration. This method seems to have possibilities for clinical use.
Kojima
T
T
Department of Legal Medicine, Hiroshima University School of Medicine, Japan.
Taniguchi
T
T
Yashiki
M
M
Miyazaki
T
T
Iwasaki
Y
Y
Mikami
T
T
Ohtani
M
M
D000328:Adult; D000368:Aged; D001463:Barbiturates / Q000008:administration & dosage / Q000493:pharmacokinetics*; D001926:Brain Death / Q000175:diagnosis / Q000503:physiopathology*; D002138:Calibration; D002648:Child; D002675:Child, Preschool; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D007262:Infusions, Intravenous; D008297:Male; D008875:Middle Aged; D012015:Reference Standards; D012631:Secobarbital / Q000008:administration & dosage / Q000493:pharmacokinetics
D001463:Barbiturates; D012631:Secobarbital; C084828:allobarbital