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  • 标题:Frit-FAB LC-MSによるスキサメトニウムの分析とラット臓器からの検出期間について
  • 本地全文:下载
  • 作者:土橋 均 ; 西川 眞弓 ; 辰野 道昭
  • 期刊名称:Journal of Health Science
  • 印刷版ISSN:1344-9702
  • 电子版ISSN:1347-5207
  • 出版年度:1997
  • 卷号:43
  • 期号:2
  • 页码:108-113
  • DOI:10.1248/jhs1956.43.108
  • 出版社:The Pharmaceutical Society of Japan
  • 摘要:The analytical procedure and detectable period of a muscular relaxant, suxamethonium, in postmortem rat tissues were studied. Rats were killed by intraperitoneal administration of suxamethonium at doses of 10 mg/kg body weight. The dead rats were stored at room temperature (25°C) and in refrigerator (0°C) until the time of the analysis. Suxamethonium in the tissues was identified and quantitated using Frit-FAB LC-MS following the solid phase extraction with a Bond Elut CBA cartridge. The rat tissue was homogenized and deproteinized with perchloric acid. The resulting supernatant was applied to the cartridge. Suxamethonium adsorbed on the cartridge was eluted with 1 ml of 0.1 M hydrochloride-methanol (1 : 1, v/v). Hexamethonium solution was added to the eluate as an internal standard. An aliquot (1 μl) of the eluate was injected into the Frit-FAB LC-MS system. The LC column used was a capillary-type Develosil ODS-UG-5 (0.3 mm i.d.×150 mm). The gradient mobile phase system was composed of eluent A (0.1% trifluoroacetic acid, including 0.4% glycerol) and eluent B (methanol, including 0.4% glycerol), and the concentration of eluent B increased from 0% to 30% over 20 min. The flow rate was 5 μl/min. The mass spectrum of suxamethonium gave the adduct of a molecular ion with trifluoroacetic acid (m/z 403) as a base peak. The detection limit of suxamethonium in the tissue by selected ion monitoring (SIM) was 5 ng/g. Suxamethonium in rats stored at 25°C and 0°C after death were found to be detectable for 7 and 42 d in the liver, 7 and 42 d in the kidney, and 2 and 4 d in the heart, respectively.
  • 关键词:suxamethonium;LC-MS;Frit-FAB;rat tissue;detectable period
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