Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Screening method for amines by derivatization reaction on TLC

TLC 상 유도체화 반응을 이용한 아민 계 화합물의 Screening 방법

  • Choi, Sung-Woon (Department of Scientific Criminal Investigation, Chungnam National University) ;
  • Lee, Hye-In (Department of Scientific Criminal Investigation, Chungnam National University) ;
  • Sung, Nack-Do (Department of Scientific Criminal Investigation, Chungnam National University)
  • 최성운 (충남대학교 평화안보대학원 과학수사학과) ;
  • 이혜인 (충남대학교 평화안보대학원 과학수사학과) ;
  • 성낙도 (충남대학교 평화안보대학원 과학수사학과)
  • Received : 2013.03.18
  • Accepted : 2013.06.28
  • Published : 2013.08.25
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Abstract

Methamphetamine is an amine-containing illegal drug and is distributed unlawfully in South Korea. Finding a rapid, convenient and semi-quantitative determination method for methamphetamine is a very important issue in the area of forensic drug testing. As an effort to develop new screening method, the reactions between three organic compounds which are structurally similar to methamphetamine and N-(9-fluorenylmethoxycarbonyloxy) succinimide (FMOC-NHS) were performed on silica gel ($SiO_2$) TLC plates. Three reference compounds were synthesized and used for the identification, comparison and study of the limit of detection (LOD) of the products obtained from a direct reaction on a TLC plate. As a result, FMOC-NHS as a derivatization reagent generated compounds containing highly UV-active functional groups on the TLC plate after reacting with primary- and secondary amines. In the experiment 2D the LOD of amines was in the range of 0.045 and 0.01 mg/mL ($2{\mu}L/spot$), and in 1D the LOD was in the range of 0.002 and 0.007 mg/mL ($2{\mu}L/spot$). The LODs of the compounds tested were dependent on the concentration of the derivatizing reagent.

국내에서 불법 유통 되거나 남용되고 있는 methamphetamine은 아민을 함유한 불법약물로서 그에 대한 신속하고 용이한 동정 및 정량적인 분석 방법은 불법약물 검사의 중요한 이슈가 되어왔다. 새로운 screening방법을 모색하기 위해 methamphetamine과 구조적으로 유사한 3종의 유기 화합물을 silica gel ($SiO_2$) TLC상에서 N-(9-Fluorenylmethoxycarbonyloxy)succinimide (FMOC-NHS)와 반응을 시켰다. TLC상 반응 생성물을 일반 유기합성 경로로 합성한 대조물질과 비교 확인한 다음, 이 방법의 검출한계(Limit of detection)를 조사하였다. 실험결과 유도체화 시약으로 사용한 FMOC-NHS는 TLC상에서 1차 및 2차 아민과 반응하여 UV-active한 화합물을 생성시키는 것을 확인하였다. 2D TLC 실험에서는 0.045-0.01 mg/mL ($2{\mu}L$ per spot), 그리고 1D co-spot TLC 실험에서 0.002-0.007 mg/mL ($2{\mu}L$ per spot)의 검출한계는 유도체화 시약의 농도에 대한 의존성을 나타내었다.

Keywords

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