SPE 및 GC/MS에 의한 혈액중 스트리크닌의 분석법 개발 및 검출사례

Method Development and Validation of Strychnine in Blood by Gas Chromatography/Mass Spectrometry Using Solid Phase Extraction and its Application in Real Specimens

  • 이종숙 (국립과학수사연구원 법과학부 약독물과) ;
  • 염혜선 (국립과학수사연구원 법과학부 약독물과) ;
  • 문성민 (국립과학수사연구원 법과학부 약독물과) ;
  • 이상기 (국립과학수사연구원 법과학부 약독물과)
  • Rhee, Jongsook (Drug & Toxicology Div., Forensic Science Dept., National Forensic Service) ;
  • Yum, Hyesun (Drug & Toxicology Div., Forensic Science Dept., National Forensic Service) ;
  • Moon, Sungmin (Drug & Toxicology Div., Forensic Science Dept., National Forensic Service) ;
  • Lee, Sangki (Drug & Toxicology Div., Forensic Science Dept., National Forensic Service)
  • 투고 : 2012.11.12
  • 심사 : 2013.03.25
  • 발행 : 2013.04.30

초록

An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.

키워드

참고문헌

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