YAKHAK HOEJI (약학회지)

The Pharmaceutical Society of Korea (대한약학회)
권호 표지

Simultaneous Analysis of 17 Organophosphorous Pesticides in Blood by Automated Head Space-SPME GC/MS

HS-SPME-GC/MS에 의한 혈액중 17종 유기인계 농약의 동시분석법

  • Rhee, Jong-Sook (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Jung, Jin-Mi (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Lee, Han-Sun (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Yeom, Hye-Sun (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Lee, Sang-Ki (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Park, Yoo-Sin (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service) ;
  • Chung, Hee-Sun (Drug & Toxicology Analysis Div., Forensic Science Dept., National Forensic Service)
  • 이종숙 (국립과학수사연구소 법과학부 약독물과) ;
  • 정진미 (국립과학수사연구소 법과학부 약독물과) ;
  • 이한선 (국립과학수사연구소 법과학부 약독물과) ;
  • 염혜선 (국립과학수사연구소 법과학부 약독물과) ;
  • 이상기 (국립과학수사연구소 법과학부 약독물과) ;
  • 박유신 (국립과학수사연구소 법과학부 약독물과) ;
  • 정희선 (국립과학수사연구소 법과학부 약독물과)
  • Received : 2010.08.16
  • Accepted : 2010.10.08
  • Published : 2010.12.31
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Abstract

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

Keywords

References

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