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  • 标题:LC/APCI-MSによるオキサゼパムグルクロナイドの分析
  • 本地全文:下载
  • 作者:辰野 道昭 ; 西川 真弓 ; 片木 宗弘
  • 期刊名称:Journal of Health Science
  • 印刷版ISSN:1344-9702
  • 电子版ISSN:1347-5207
  • 出版年度:1992
  • 卷号:38
  • 期号:2
  • 页码:162-167
  • DOI:10.1248/jhs1956.38.162
  • 出版社:The Pharmaceutical Society of Japan
  • 摘要:A high performance liquid chromatography-mass spectrometric (LC-MS) method for the determination of oxazepam glucuronide in the human urine was investigated. Oxazepam glucuronide was extracted from the urine by using Sep-Pak C18 cartridge with methanol-50 mM ammonium acetate (70 : 30 v/v) as eluent. The eluate was analyzed by LC-MS equipped with atmospheric pressure chemical ionization (APCI). High performance liquid chromatographic (HPLC) analyses were performed on a L-column (C18 reversed phase column) in the solvent system of methanol-50 mM ammonium acetate (70 : 30 v/v) at a flow rate of 1.0 ml/min. The vaporizer temperature was set to 230°C, desolvation temperature to 390°C, drift voltage to 108V, focus voltage to 96V and multiplier voltage to 2400V. Peak areas were measured using selected ion monitoring (SIM) of a base ion peak at m/z 287. The calibration curve gave a good linearity over the range of 0.25-1 μl/ml. The detection limit was 50 ng/ml by recording the base ion peak at m/z 287.
  • 关键词:oxazepam glucuronide;LC/APCI-MS;Sep-Pak C18 cartridge;SIM;human urine
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