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Development of rapid and sensitive methods for the forensic analysis of xenobiotic substances in hair

Research Project

Project/Area Number 23615011
Research Category

Grant-in-Aid for Scientific Research (C)

Allocation TypeMulti-year Fund
Section一般
Research Field Reliable environmental measurement methods
Research InstitutionNational Research Institute of Police Science

Principal Investigator

MIYAGUCHI Hajime  科学警察研究所, 附属鑑定所, 主任研究官 (10370884)

Project Period (FY) 2011 – 2013
Project Status Completed (Fiscal Year 2013)
Budget Amount *help
¥4,680,000 (Direct Cost: ¥3,600,000、Indirect Cost: ¥1,080,000)
Fiscal Year 2013: ¥1,170,000 (Direct Cost: ¥900,000、Indirect Cost: ¥270,000)
Fiscal Year 2012: ¥1,170,000 (Direct Cost: ¥900,000、Indirect Cost: ¥270,000)
Fiscal Year 2011: ¥2,340,000 (Direct Cost: ¥1,800,000、Indirect Cost: ¥540,000)
Keywords科学捜査 / 毛髪中薬物分析 / 催眠鎮静薬 / マイクロ粉砕抽出法 / 毛髪分析 / 液体クロマトグラフィー/質量分析 / ゾルピデム / ガスクロマトグラフィー/質量分析
Research Abstract

We established a new sample preparation method for the analysis of 13 sedative-hypnotics. Following micropulverized extraction with 3.0 M ammonium phosphate, a QExactive hybrid mass spectrometer was used to identify the analytes. The sample size requirement was reduced to 5 mg. The lower limits of quantification (LLOQ) were 1 pg/mg for brotizolam, diazepam, N-desmethyldiazepam, estazolam, flunitrazepam, nitrazepam, triazolam, ramelteon and zolpidem, and 4 pg/mg for alprazolam, N-desmethylfludiazepam, etizolam and zopiclone. Accuracy and precision of the repeated analyses for all the analytes met FDA guidelines at three concentrations. The developed method was applied to hair samples from four patients with sleep disorders. Compared with earlier methods, the present method requires a smaller amount of sample and is complete within a shorter analytical time. These method improvements will be helpful for detecting administration of sedative-hypnotics from hair samples of victims of DFSA.

Report

(4 results)
  • 2013 Annual Research Report   Final Research Report ( PDF )
  • 2012 Research-status Report
  • 2011 Research-status Report
  • Research Products

    (15 results)

All 2014 2013 2012

All Journal Article (3 results) (of which Peer Reviewed: 1 results) Presentation (12 results)

  • [Journal Article] Determination of sedative-hypnotics in human hair by micropulverized extraction and liquid chromatography/quadrupole-Orbitrap mass spectrometry2014

    • Author(s)
      Miyaguchi, H
    • Journal Title

      Anal Methods

      Volume: (in press (published online)) Issue: 15 Pages: 5777-5783

    • DOI

      10.1039/c4ay00505h

    • Related Report
      2013 Annual Research Report 2013 Final Research Report
  • [Journal Article] Determination of zolpidem in human hair by micropulverized extraction based on the evaluation of relative extraction efficiency of seven psychoactive drugs from an incurred human hair specimen2013

    • Author(s)
      Miyaguchi, H
    • Journal Title

      J Chromatogr A

      Volume: 1293 Pages: 28-35

    • DOI

      10.1016/j.chroma.2013.04.007

    • Related Report
      2013 Final Research Report 2012 Research-status Report
  • [Journal Article] Development of an automated and sensitive GC/MS system for the analysis of amphetamine-type stimulants in hair.2012

    • Author(s)
      杉山茂, 樋口美代子, 栁堀あや子, 宮川治彦, 井上博之
    • Journal Title

      Japanese Journal of Forensic Science and Technology

      Volume: 17 Issue: 1 Pages: 27-34

    • DOI

      10.3408/jafst.17.27

    • NAID

      130004942639

    • ISSN
      1880-1323, 1881-4689
    • Related Report
      2013 Final Research Report 2011 Research-status Report
    • Peer Reviewed
  • [Presentation] メンブレンフィルトレーションにおける薬物吸着ロスの評価2013

    • Author(s)
      宮口一, 岩田祐子
    • Organizer
      日本法科学技術学会第19回学術集会
    • Place of Presentation
      東京都港区・フロラシオン青山
    • Year and Date
      2013-11-14
    • Related Report
      2013 Final Research Report
  • [Presentation] Determination of thirteen sedative/hypnotics in human hair by micropulverized extraction and liquid chromatography/quadrupore-Orbitrap mass spectrometry2013

    • Author(s)
      H. Miyaguchi
    • Organizer
      The 11th Indo Pacific Association of Law, Medicine and Science Congress (INPALMS2013)
    • Place of Presentation
      クアラルンプール・Shangri La Hotel
    • Year and Date
      2013-10-08
    • Related Report
      2013 Final Research Report
  • [Presentation] マイクロ粉砕抽出法による毛髪中ゾルピデムの迅速定量分析2013

    • Author(s)
      宮口一
    • Organizer
      日本法中毒学会第32年会
    • Place of Presentation
      千葉県柏市・さわやかちば県民プラザ
    • Year and Date
      2013-07-05
    • Related Report
      2013 Final Research Report
  • [Presentation] メンブレンフィルトレーションにおける薬物吸着ロスの評価2013

    • Author(s)
      宮口 一,岩田祐子
    • Organizer
      日本法科学技術学会第19回学術集会
    • Place of Presentation
      フロラシオン青山(東京都港区)
    • Related Report
      2013 Annual Research Report
  • [Presentation] Determination of thirteen sedative/hypnotics in human hair by micropulverized extraction and liquid chromatography/quadrupore-Orbitrap mass spectrometry2013

    • Author(s)
      H. Miyaguchi
    • Organizer
      The 11th Indo Pacific Association of Law, Medicine and Science Congress (INPALMS2013)
    • Place of Presentation
      シャングリラホテル(マレーシア)
    • Related Report
      2013 Annual Research Report
  • [Presentation] マイクロ粉砕抽出法による毛髪中ゾルピデムの迅速定量分析2013

    • Author(s)
      宮口 一
    • Organizer
      日本法中毒学会第32年会
    • Place of Presentation
      さわやかちば県民プラザ(千葉県柏市)
    • Related Report
      2013 Annual Research Report
  • [Presentation] 毛髪中催眠薬・抗不安薬・抗うつ薬の高速抽出法の開発2012

    • Author(s)
      宮口一
    • Organizer
      日本法科学技術学会第18回学術集会
    • Place of Presentation
      東京都港区・フロラシオン青山
    • Year and Date
      2012-11-15
    • Related Report
      2013 Final Research Report
  • [Presentation] Significant acceleration of sample preparation for several psychoactive drugs in human hair by micropulverized extraction2012

    • Author(s)
      Miyaguchi, H
    • Organizer
      17th Annual Meeting of the Society of Hair Testing
    • Place of Presentation
      トロント・Hospital for Sick Children
    • Year and Date
      2012-06-26
    • Related Report
      2013 Final Research Report
  • [Presentation] Miyaguchi, H., Inoue, H., Sugiyama, H., Miyagawa, H.2012

    • Author(s)
      Identification of amphetamine-type stimulants in hair based on full scan mass spectra from a modified GC/MS system
    • Organizer
      The 50th Annual Meeting of the International Association of Forensic Toxicologist
    • Place of Presentation
      静岡県浜松市・アクトシティ浜松
    • Year and Date
      2012-06-04
    • Related Report
      2013 Final Research Report
  • [Presentation] (24) Identification of amphetamine-type stimulants in hair based on full scan mass spectra from a modified GC/MS system2012

    • Author(s)
      Miyaguchi, H., Inoue, H., Sugiyama, H., Miyagawa, H.
    • Organizer
      The 50th Annual Meeting of the International Association of Forensic Toxicologist
    • Place of Presentation
      アクトシティ浜松(浜松市)
    • Related Report
      2012 Research-status Report
  • [Presentation] (25) Significant acceleration of sample preparation for several psychoactive drugs in human hair by micropulverized extraction2012

    • Author(s)
      Miyaguchi, H.
    • Organizer
      17th Annual Meeting of the Society of Hair Testing
    • Place of Presentation
      Hospital for Sick Cilidren, Toronto
    • Related Report
      2012 Research-status Report
  • [Presentation] 毛髪中催眠薬・抗不安薬・抗うつ薬の高速抽出法の開発2012

    • Author(s)
      宮口 一
    • Organizer
      日本法科学技術学会第18回学術集会
    • Place of Presentation
      ホテルフロラシオン青山(東京都港区)
    • Related Report
      2012 Research-status Report

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Published: 2011-08-05   Modified: 2019-07-29  

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