YOSHIMURA Sumitaka Kansai Medical University, Faculty of Medicine, Assistant, 医学部, 助手 (70167005)
OKII Yutaka Kansai Medical University, Faculty of Medicine, Assistant, 医学部, 助手 (20121915)
WATABIKI Toshimitsu Kansai Medical University, Faculty of Medicine, Lecturer, 医学部, 講師 (70077692)
AKANE Atsushi Kansai Medical University, Faculty of Medicine, Professor, 医学部, 教授 (70202520)
|Budget Amount *help
¥1,700,000 (Direct Cost : ¥1,700,000)
Fiscal Year 1996 : ¥700,000 (Direct Cost : ¥700,000)
Fiscal Year 1995 : ¥1,000,000 (Direct Cost : ¥1,000,000)
Increase of acute drug toxicosis caused by accidental or deliberate overdosage of sleeping drugs or tranquilizers has become a social problem. Establishment of quick and simple analysis for diagnosis of the toxicosis is thus required. In this research, rapid determination of the drugs by flow injection-thermospray mass spectrometry was investigated.
Under the thermospray ionization mode and the filament-on ionization mode, MH^+ ions of most of the standard drugs were detected as base peaks. A semi-automatic drug extraction system was also applied, which consisted of Sep-Pak tCl8 column and a peristaltic pump controlled by personal computer, resulting in high reproduction rates.
Gastric contents, which may contain large amounts of administered drugs, were expected to be the most suitable specimens for analysis. As the pretreatment, an equal volume of distillled water, ethanol or acetonitrile was added into the specimens, followed by centrifugation at 3,000rpm for 10 min. Drugs were extrac
ted with ethyl acetate from the supernatants. When gastric contents containing no drugs were not pretealed, impurity ions were detected to some extent. Pretreatment with ethanol or acetonitrile enhanced intensities of the ions, interfering with the analysis. When gastric contents containing 1mug/ml benzodiazepines and dihydrocodeine were assayd, the drugs could not be detected well from non-pretreated samples but from samples treated with distillled water. Therefore, pretreatment with distillled water was most suitable for the determination.
Since such drugs might be detected as ions of the same molecular weight, identification of each drug from their mixture by flow injection method would be difficult in some cases. To improve it, a simple separation column (a 1/16 inch * 1.0mm * 20 cm stainless-steel tube packed with Sep-Pak C18) was combined prior to the analysis system. The mobile phase used was acetonitrile-water (40 : 60, v/v) containing 0.1M ammonium acetate. By this modification, peaks representing the drugs were separated at retention time ranged 0.4-1.2 min, and each drug could be detected even from non-pretreated gastric contents containing the drugs. In combination with drug screening test devices such as Triage and Visualine, the flow injection method is a powerful measure for the rapid drug identification. Less