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HPLC/MS of Antibiotics in Biological Samples

Research Project

Project/Area Number 09670454
Research Category

Grant-in-Aid for Scientific Research (C)

Allocation TypeSingle-year Grants
Section一般
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.Sch.Med., Research Associate, 医学部, 助手 (30266085)
LEE Xiao-pen  Showa Univ.Sch.Med., Research Associate, 医学部, 助手 (90245829)
Project Period (FY) 1997 – 1998
Project Status Completed (Fiscal Year 1998)
Budget Amount *help
¥3,600,000 (Direct Cost: ¥3,600,000)
Fiscal Year 1998: ¥900,000 (Direct Cost: ¥900,000)
Fiscal Year 1997: ¥2,700,000 (Direct Cost: ¥2,700,000)
KeywordsLiquid Chromatography / Mass Spectrometry / Fast Atom Bombardment / Antibiotics / Cephem Antibiotics / Aminoglycoside Antibiotics / Ion-pair HPLC / Solid-Phase Extraction / 固相抽出 / イオンベアー逆相HPLC / 薬物ショック死
Research Abstract

We analyzed two representative antibiotics, cephems and aminoglycosides, by our recently established system of capillary high-performance liquid chromatography (HPLC)/fast atom bombardment (FAB)-mass spectrometry (MS). Cephems could be analyzed by conventional reversed-phase HPLC, but aminoglycosides required ion-pair reversed-phase HPLC.As a matrix for FAB-MS, diethanolamine (DEA) along with glycerin (GLY) were used. The authentic compounds of 24 cephems and 8 aminoglycosides were analyzed by our capillary HPLC/FAB-MS system. Whend a suitable matrix was used for each antibiotic, quasi-molecular peak together with adequate fragment peaks were obtained from all 32 antibiotics, though DEA provided more information on molecular mass of a compound than did GLY for some cephems. The range of the detection limits of the mass spectral measurements was rather wide (10 ng - 2.5 mug on column), but sufficiently sensitive to detect therapeutic levels of antibiotics in human serum for most compounds under investigation.
The extraction of the antibiotics from human serum was studied using solid-phase extraction cartridges. In general, Bond Elut C_<18> cartridges were effective for the isolation of cephems and aminoglycosides under investigation. With this isolation procedure and the capillary HPLC/FAB-MS in the positive mode, cefazolin and ribostamycin, representative cephem antibiotic and aminoglycoside, respectively, could be identified in sera from cadavers who suddenly died after injection of them. The capillary HPLCIFAB-MS was semi-quantitative for all compounds under investigation. However, we believe that accurate quantifation can be made by SIM of FAB-MS with a suitable isotopic internal standard. We also devised a simple method for quantitation of some other drugs in human serum by UV monitoring of the capillary HPLC.
These analytical methods devised in this study would seem to be useful in clinical pharmacology as well as in forensic toxicology.

Report

(3 results)
  • 1998 Annual Research Report   Final Research Report Summary
  • 1997 Annual Research Report
  • Research Products

    (35 results)

All Other

All Publications (35 results)

  • [Publications] Takeshi Kumazawa: "Extraction of cocaine in human urine by direct immersion-solid phase micro extraction(SPME)" Advances in Legai Medicine. 3. 485-488 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Keizo Sato: "Capillary HPLC/FAB-MS of 24 cephem antibiotics" Advances in Legal Medicine. 3. 538-542 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "A new analysis of organophosphate pesticides in human body fluids by headspace solid-phase micro extraction" Advances in Legal Medicine. 3. 543-547 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "A new extraction of thinner components in human body fluids by headspace solid-phase micro extraction(SPME)before capillary gas chromatography" Current Topics in Forensic Science. 2. 220-223 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Toshiyuki Sano: "Quantitation of midazolam in serum by column-switching capillary HPLC/FAB-MS using a deuterium-labeled internal standard" Current Topics in Forensic Science. 2. 235-236 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Keizo Sato: "Analyses of phenothiazines by capillary high-performance liquid chromatography/fast atom bombardment-mass spectrometry" Current Topics in Forensic Sciemce. 2. 348-351 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Detection of cresol isomers and phenol in human whole blood by headspace solid-phase micro extraction(SPME)and capillary gas chromatography" Jpn.J.Forensic Toxicol. 15. 21-28 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Detection of tricyclic antidepressants in whole blood by headspace solid-phase microextraction and capillary gas chromatography" J.Chromatogr.Sci. 35. 302-308 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Determination of solvent thinner components in human body fluids by capillary gas chromatography with trapping at low oven temperature for headspace samples" Analyst. 123. 147-150 (1998)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Simple extraction of methanol in human whole blood by headspace solid-phase microextraction(SPME)" Jpn.J.Forensic Toxicol. 16. 64-68 (1998)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Improved extraction of ethanol from human body fluids by headspace solid-phase microextraction with a carboxen-polydimethylsiloxane-coated fiber" Chromatographia. 47. 593-595 (1998)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Tomoko Taguchi: "High-performance liquid chromatographic determination of benzodiazepines in serum with 0.3 mm I.D. columns" 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. 6. 781-784 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Simple extraction of alcohols in human body fluids by headspace solid-phase microextraction(SPME)" 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. 6. 820-823 (1999)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] T.Kumazawa, K.Watanabe, X.-P.Lee, K.Sato, and O.Suzuki: "Extraction of cocaine in human urine by direct immersion-solid phase micro extraction (SPME)." Advances in Legal Medicine. 3. 485-488 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] K.Sato, K.Kobayashi, X.-P.Lee, S.Furuta and Y.Katsumata: "Capillary HPLC/FAB-MS of 24 cephem antibiotics." Advances in Legal Medicine. 3. 538-542 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, K.Sato and O.Suzuki: "A new analysis of organophosphate pesticides in human body fluids by headspace solid-phase micro extraction." Advances in Legal Medicine. 3. 543-547 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa and K.Sato: "A new extraction of thinner components in human body fluids by headspace solid-phase micro extraction (SPME) before capillary gas chromatography." Current Topics in Forensic Science. 2. 220-223 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] T.Sano, K.Sato, K.Kobayashi, Y.Mizuno and Y.Katsumata: "Quantitation of midazolam in serum by column-switching capillary HPLC/FAB-MS using a deuterium-labeled internal standard." Current Topics in Forensic Science. 2. 235-236 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] K.Sato, Y.Mizuno, X.-P.Lee, T.Taguchi and Y.Katsumata: "Analyses of phenothiazines by capillary high-performance liquid chromatography/fast atom bombardment-mass spectrometry." Current Topics in Forensic Science. 2. 348-351 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, S.Furuta, T.Kurosawa, K.Akiya, I.Akiya and K.Sato: "Detection of cresol isomers and phenol in human whole blood by headspace solid-phase micro extraction (SPME) and capillary gas chromatography." Jpn.J.Forensic Toxicol.15. 21-28 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, K.Sato and O.Suzuki: "Detection of tricyclic antidepressants in whole blood by headspace solid-phase microextraction and capillay gas chromatography." J.Chromatogr.Sci.35. 302-308 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, K.Sato, K.Watanabe, H.Seno and O.Suzuki: "Determination of solvent thinner components in human body fluids by capillary gas chromatography with trapping at low oven temperature for headspace samples." Analyst. 123. 147-150 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa T.Kurosawa, K.Akiya, Y.Akiya, S.Furuta and K.Sato: "Simple extraction of methanol in human whole blood by headspace solid-phase microextraction (SPME)." Jpn.J.Forensic Toxicol.16. 64-68 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, K.Sato, H.Seno, A.Ishii and O.Suzuki: "Improved extraction of ethanol from human body fluids by headspace solid-phase microextraction with a carboxen-polydimethylsiloxane-coated fiber." Chromatographia. 47. 593-595 (1998)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] T.Taguchi, K.Akiya, X.-P.Lee, T.Kumazawa, Y.Akiya and K.Sato: "High-performance liquid chromatographic determination of benzodiazepines in serum with 0.3mm I.D.columns." 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. 6. 781-784 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] X.-P.Lee, T.Kumazawa, T.Taguchi, S.Furuta, K.Sato, A.Ishii, H.Seno and O.Suzuki: "Simple Extraction of Alcohols in Human Body Fluids by Headspace Solid-Phase Microextraction (SPME)." 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. 6. 820-823 (1999)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1998 Final Research Report Summary
  • [Publications] Xiao-Pen Lee: "Improved extraction of ethanol from human body fluids by headspace solid-phase microextraction with a carboxen-polydimethylsiloxane-coated fiber" Chromatographia. 47. 593-595 (1998)

    • Related Report
      1998 Annual Research Report
  • [Publications] Tomoko Taguchi: "High-performance liquid chromatographic determination of benzodiazepines in serum with 0.3mm I.D.columns" Proceedings of the 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. (in press).

    • Related Report
      1998 Annual Research Report
  • [Publications] Xiao-Pen Lee: "Simple extraction of alcohols in human body fluids by headspace solid-phase microextraction(SPME)." Proceedings of the 6th Indo Pacific Congress on Legal Medicine and Forensic Sciences. (in press).

    • Related Report
      1998 Annual Research Report
  • [Publications] Keizo Sato: "Capillary HPLC/FAB-MS of 24 cephem antibiotics" Advances in Legal Medicine. 3. 538-542 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Takeshi Kumazawa: "Extraction of cocaine in human urinr by direct immersion-solid phase micro extraction(SPME)" Advances in Legal Medicine. 3. 485-488 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Xiao-Pen Lee: "A new analysis of organophosphatepesticides in human body fluids by headspace solid-phase micro extraction" Advances in Legal Medicine. 3. 543-547 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Xiao-Pen Lee: "Detection of tricyclic antidepressants in whole blood by headspace solid-phase microextraction and capillary gas chromatography" Journal of Chromatgraphic Science. 35. 302-308 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Xiao-Pen Lee: "Determination of solvent thinner components in human body fluids by capillary gas chromatography with trapping at low oven temperature for headspace samples" Analyst. 123. 147-150 (1998)

    • Related Report
      1997 Annual Research Report
  • [Publications] Xiao-Pen Lee: "Simple extraction of methanol in human whole blood by headspace solid-phase microextraction(SPME)" Japanese Journal of Forensic Toxicology. 16. 64-68 (1998)

    • Related Report
      1997 Annual Research Report

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Published: 1997-04-01   Modified: 2016-04-21  

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