Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Simultaneous determination of amphetamine-like drugs in human urine by SPE and GC/MS

고체상추출과 GC/MS를 이용한 소변 중 암페타민계 마약성분 동시분석법

  • Cheong, Jae Chul (Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office) ;
  • Kim, Jin Young (Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office) ;
  • In, Moon Kyo (Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office) ;
  • Cheong, Won Jo (Department of Chemistry, Inha University)
  • Received : 2007.08.28
  • Accepted : 2007.11.19
  • Published : 2008.02.25
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Abstract

Although liquid-liquid extraction (LLE) method has been used routinely for the analysis of amphetamine-like drugs (amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA), a solid-phase extraction (SPE) method, which can be automated, was applied for the simultaneous determination by GC/MS in human urine. Urine samples (3 mL) and 0.1 M phosphate buffer (1 mL, pH 7.0) were extracted by an automated SPE system. The eluent was evaporated, derivatized with trifluoroacetic anhydride (TFAA), and analyzed by GC/MS. The calibration curves was linear with correlation coefficient ($r^2$) above 0.994 in the ranges of 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL for AP, MDA, and 50.0~2000.0 ng/mL for MA, MDMA, and MDEA. The limits of detection ranged from 4.0 to 10.0 ng/mL, and the limits of quantitation ranged from 12.0 to 34.0 ng/mL. The relative recoveries were 93.5~107.7 %. The precisions and accuracies were 1.9~14.8 % and -8.7~14.8 %, respectively. The present method was successfully applied to identify the MA or Ecstasy (MDMA) abusers in exact as well as rapid.

소변 중 암페타민계 5성분(amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA)의 동시분석을 위하여 기존의 액체상추출(liquid-liquid extraction; LLE) 방법과는 달리 감정과정의 자동화가 가능한 고체상추출(solid-phase extraction, SPE) 방법을 도입하였다. 시험관에 소변 3 mL와 0.1 M 인산완충액 1 mL (pH 7.0)를 넣고, 자동추출장치를 이용하여 추출하고, 증발 건고하여 유도체화 한 다음 GC/MS로 분석하였다. 그 결과 검정곡선의 직선성 상관계수 ($r^2$)는 AP와 MDA [농도범위 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL] 및 MA, MDMA, MDEA (농도범위 50.0~2000.0 ng/mL)에서 0.994 이상으로 나타났다. 그리고 각 성분들의 검출한계 (LOD)는 4.0~10.0 ng/mL 범위였고, 정량한계 (LOQ)는 12.0~34.0 ng/mL 범위였다. 상대 회수율은 5성분 모두 93.5~107.7%로 측정되었다. 정밀도 (precision)와 정확도 (accuracy)는 각각 1.9~14.8%와 -8.7~14.8 % 범위 값을 나타냈다. 본 실험방법을 실제 남용자 소변에 적용한 결과 메스암페타민 또는 엑스터시 투약자를 신속하고 정확하게 동시에 확인할 수 있었다.

Keywords

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