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High-Performance Liquid Chromatography/Mass Spectrometry of Psychotropic Drugs

Research Project

Project/Area Number 06670469
Research Category

Grant-in-Aid for General Scientific Research (C)

Allocation TypeSingle-year Grants
Research Field Legal medicine
Research InstitutionShowa University

Principal Investigator

SATO Keizo  Showa Univ.Sch.Med., Professor, 医学部, 教授 (20162422)

Co-Investigator(Kenkyū-buntansha) TAGUCHI Tomoko  Showa Univ.School of Medicine, Research Associate, 医学部, 助手 (30266085)
LEE Xiao-pen  Showa Univ.School of Medicine, Research Associate, 医学部, 助手 (90245829)
DOGE Koichi  Showa Univ.School of Medicine, Assistant Professor, 医学部, 講師 (60188844)
KUMAZAWA Takeshi  Showa Univ.School of Medicine, Associate Professor, 医学部, 助教授 (00186470)
Project Period (FY) 1994 – 1995
Project Status Completed (Fiscal Year 1995)
Budget Amount *help
¥2,100,000 (Direct Cost: ¥2,100,000)
Fiscal Year 1995: ¥500,000 (Direct Cost: ¥500,000)
Fiscal Year 1994: ¥1,600,000 (Direct Cost: ¥1,600,000)
KeywordsLiquid Chromatography / Mass Spectrometry / Fast Atom Bombardment / Psychotropic Drugs / Benzodiazepines / Phenothiazines / Butyrophenones / Solid-Phase Extraction / 固相抽出 / プチロフェノン
Research Abstract

We analyzed three representative psychotropic drugs, benzodiazepines, phenothiazines and butyrophenones, by our recently established system of capillary high-performance liquid chromatography (HPLC) /fast atom bombardment (FAB) -mass spectrometry (MS). The authentic compounds of 27 benzodiazepines, 17 phenothiazines and 6 butyrophenones were analyzed by the system. Quasi-molucular peaks along with adequate fragment peaks were detected in the positive mode for most compounds under investigation with the detection limit of less than 10ng on columun. Sensitivity in the nagative mode with respect to its mass spectral measurement was two order of magnitude lower than that in the positive mode.
The extraction of the drugs from human blood or urine was studied using various solid-phase extraction cartridges. In general, C_<18> cartridges were effective for the isolation of benzodiazepines, C_2 cartridges for that of phenothiazines or butyrophenones. With this isolation procedure and the capillary HPLC/FAB-MS in the positive mode, some representative benzodiazepines or phenothiazines together with their metabolites could be identified in human sera after oral administration of them.
We established a method for quantitative analysis of the concentration of midazolam, one of representative benzodiazepines, in serum by selected ion-monitoring (SIM) of FAB-MS, using deuterium-labeled midazolam as an internal standard. The calibration graph was linear for concentrations between 2ng/ml and 200ng/ml, and reproducibility was good. The capillary HPLC/FAB-MS was semi-quantitative for all compounds under investigation. However, we feel that accurate quantitation can be made by SIM of FAB-MS with a suitable isotopic internal standard. We also devised a simple method for quantitation of some benzodiazepines in human serum by UV monitoring of the capillary HPLC.
These analytical methods devised in this study would seen to be useful in clinical pharmacology as well as in forensic toxicology.

Report

(3 results)
  • 1995 Annual Research Report   Final Research Report Summary
  • 1994 Annual Research Report
  • Research Products

    (27 results)

All Other

All Publications (27 results)

  • [Publications] Takeshi Kumazawa: "Positive and negative ion mass spectrometry of ten xanthine derivatives and their rapid clean-up with Sep-pak C_<18> cartridges from biological samples" Forensic Sci.Int.68. 53-67 (1994)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Keizo Sato: "On-line high-performance liquid chromatography-fast atom bombardment mas spectrometry in forensic analysis" J.Chromatogr.A. 674. 127-145 (1994)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Positive and negative-ion mass spectrometry of seven dinitroaniline herbicides" Jpn.J.Forensic Toxicol.12. 228-240 (1994)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Simple extraction of tricyclic antidepressants in human urine by headspace solid-phase microextraction (SPME)" Jpn.J.Forensic Toxicol.13. 25-30 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Rapid extraction and capillary gas chromatography for diazine herbicides in human body fluids" Forensic Sci.Int.72. 199-207 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Capillary gas chromatography with four different detectors for dinitroaniline herbicides in human body fluids" J.Anal.Toxicol.19. 95-98 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "A simple analysis of 5 thinner components in human body fluids by headspace solid-phase microextraction (SPME)" Int.J.Legal Med.107. 310-313 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Detection of ten local anaesthetics in human blood using solid-phase microextraction (SPME) and capillary gas chromatography" Jpn.J.Forensic Toxicol.13. 182-188 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Detection of cocaine in human urine by solid-phase microextraction and capillary gas chromatography with nitrogen-phosphorus detection" Jpn.J.Forensic Toxicol.13. 207-210 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, K.Sato, H.Seno, A.Ishii and O.Suzuki: "Positive and negative ion mass spectrometry of ten xanthine derivatives and their rapid clean-up with Sep-Pak C_<18> cartridges from biological samples" Forensic Sci.Int.68. 53-67 (1994)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] K.Sato, T.Kumazawa and Y.Katsumata: "On-line high-performance liquid chromatography-fast atom bombardment mass spectrometry in forensic analysis" J.Chromatogr.A. 674. 127-145 (1994)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, K.Sato, H.Seno, A.Ishii and O.Suzuki: "Positive and negative-ion mass spectrometry of seven dinitroaniline herbicides" Jpn.J.Forensic Toxicol.12. 228-240 (1994)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, X.-P.Lee, M.-C.Tsai, H.Seno: "A.Ishii and K.Sato, Simple extraction of tricyclic antidepressants in human urine by headspace solid-phase microextraction (SPME)" Jpn.J.Forensic Toxicol.13. 25-30 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa and K.Sato: "Rapid extraction and capillary gas chromatography for diazine herbicides in human body fluids" Forensic Sci.Int.72. 199-207 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, K.Sato, H.Seno: "A.Ishii and O.Suzuki, Capillarygas chromatography with four different detectors for dinitroaniline herbicides in human body fluids" J.Anal.Toxicol.19. 95-98 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa and K.Sato: "A simple analysis of 5 thinner components in human body fluids by headapace solid-phase microextraction (SPME)" Int.J.Legal Med.107. 310-313 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, X.-P.Lee, K.Sato, H.Seno, A.Ishii and O.Suzuki: "Detection of ten local anaesthetics in human blood using soild-phase microextraction (SPME) and capillary gas chromatography" Jpn.J.Forensic Toxicol.13. 182-188 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] T.Kumazawa, K.Watanabe, K.Sato, H.Seno, A.Ishii and O.Suzuki: "Detection of cocaine in human urine by solid-phase microextraction and capillary gas chromatography with nitrogenphosphorus detection" Jpn.J.Forensic Toxicol.13. 207-210 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] Takeshi Kumazawa: "Positive and negative-ion mass spectrometry of seven dinitroaniline herbicides" Jpn. J. Forensic Toxicol.,. 12. 228-240 (1994)

    • Related Report
      1995 Annual Research Report
  • [Publications] Xiao-Pen Lee: "Rapid extraction and capillary gas chromatography for diazine herbicides in human body fluids" Forensic Sci. Int.,. 72. 199-207 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Capillary gas chromatography with four different detectors for dinitroaniline herbicides in human body fluids" J. Anal. Toxicol.,. 19. 95-98 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Xiao-Pen Lee: "A simple analysis of 5 thinner components in human body fluids by headspace solid-phase microextraction (SPME)" Int. J. Legal Med.,. 107. 310-313 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Detection of ten local anaesthetics in human blood using solid-phase microextraction (SPME) and capillay gas chromatography" Jpn. J. Forensic Toxicol.,. 13. 182-188 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Detection of cocaine in human urine by solid-phase microextraction and capillary gas chromatography with nitrogen-phosphorus detection" Jpn. J. Forensic Toxicol.,. 13. 207-210 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Keizo Sato: "On-line high-performance liquid chromatography-fast atom bombardment mass spectrometry in forensic analysis" Journal of Chromatography A. 674. 127-145 (1994)

    • Related Report
      1994 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Positive and negative ion mass spectrometry of ten xanthine derivatives and their rapid clean-up with Sep-pak C^<18> cartridges from biological samples" Forensic Science International. 68. 53-67 (1994)

    • Related Report
      1994 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Simple extraction of tricyclic antidepressants in human urine by headspace solid-phase microextraction(SPME)" Japanese Journal of Forensic Toxicology. 13(in-press). (1995)

    • Related Report
      1994 Annual Research Report

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Published: 1994-04-01   Modified: 2016-04-21  

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