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

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タイトル別名
  • The Analytical Procedure by Frit-FAB LC-MS and Detectable Period of Suxamethonium in Rats Tissues.
  • Frit-FAB LC-MS ニヨル スキサメトニウム ノ ブンセキ ト ラッ

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抄録

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.

収録刊行物

  • 衛生化学

    衛生化学 43 (2), 108-113, 1997

    公益社団法人 日本薬学会

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