Environmental Analysis Health and Toxicology

The Korean Society of Environmental Health and Toxicology (환경독성보건학회)
권호 표지

Method Validation for the Simultaneous Analysis of Organophosphorous Pesticides in Blood by GC/MS

GC/MS를 이용한 혈액 중 유기인제류 농약의 동시 분석에 관한 방법의 유효화

  • Park Mee Jung (Forensic Science Department, National Institute of Scientific investigation) ;
  • Yang Ja Youl (Forensic Science Department, National Institute of Scientific investigation) ;
  • Kim Ki Wook (Forensic Science Department, National Institute of Scientific investigation) ;
  • Park Yoo Shin (Forensic Science Department, National Institute of Scientific investigation) ;
  • Chung Hee Sun (Forensic Science Department, National Institute of Scientific investigation) ;
  • Lee Sang Ki (Forensic Science Department, National Institute of Scientific investigation)
  • 박미정 (국립과학수사연구소 법과학부) ;
  • 양자열 (국립과학수사연구소 법과학부) ;
  • 김기욱 (국립과학수사연구소 법과학부) ;
  • 박유신 (국립과학수사연구소 법과학부) ;
  • 정희선 (국립과학수사연구소 법과학부) ;
  • 이상기 (국립과학수사연구소 법과학부)
  • Published : 2005.12.01
Download PDF
⟨ Previous Next ⟩

Abstract

The purpose of this study was to provide the standard method for the analysis of organophosphorous pesticides such as chlorpyrifos, diazinon, malathion and parathion in blood. We performed method validation for these pesticides in blood according to EURACHEM (A focus For Analytical Chemistry in Europe) guide. For the analysis of the pesticides, we used solid-phase extraction ,column (Waters Oasis $HLB^{(R)}$. After the extraction, the supernatants were evaporated to dryness under the nitrogen stream. They were analyzed by gas chromatography/mass spectrometry (GC/MS) after reconstituting with ethanol. Terbufos was used as an internal standard. To validate this method, we performed verification procedures with the following parameters: selectivity, linearity of calibration, accuracy, precision, limit of detection and quantification. Validation data according to Eurachem guide were adequate for our purpose for the analysis of chlorpyrifos, diazinon, malathion and parathion in blood.

Keywords

References

  1. 김기욱, 양자열, 이수연, 이상기. HS-SPME를 이용한 생체시료 중 유기인제류 농약의 동시분석, 국립과학수사연구소 연보. 2003; 35: 259-264
  2. Barroso M, Gallardo E, Margalho C, Marques E, Vieira DN and Lopez-Rivadulla M. Determination of strychnine in human blood using solid-phase extraction and GC-EIMS, J Anal Toxicol 2005; 29(5): 383-386 https://doi.org/10.1093/jat/29.5.383
  3. Frank M, Heike H and Burhard M. Simple determination of 22 organophosphorous pesticides in human blood using headspace solid-phase microextraction and gas chromatography with mass spectrometric determination, J Chromatogr Sci 2002; 40: 29-34 https://doi.org/10.1093/chromsci/40.1.29
  4. Goncalves G and Alpendurada MF. Multiresidue method for the simultaneous determination of four groups of pesticides in ground and drinking waters, using solid-phase microextraction-gas chromatography with electroncapture and thermionic specific detection, J Chromatogr A 2002; 968: 177-190 https://doi.org/10.1016/S0021-9673(02)00788-4
  5. Guide to Quality in Analytical Chemistry, An Aid to Accreditation. Eurachem (A focus For Analytical Chemistry in Europe), 2002
  6. Hercegova A, Domotorova M, Matisova E, Kirchner M, Otrekala R and Stefuca V. Fast gas chromatography with solid phase extraction clean-up for ultratrace analysis of pesticide residues in baby food, J Chromatogr A 2005; 1084(1-2): 46-53 https://doi.org/10.1016/j.chroma.2004.10.108
  7. Luca A, Francesco B, Anna S, Carollo DL and Lelio Z. Analysis of organophosphorus pesticides by gas chromatography-mass spectrometry with negative chemical ionization: a study on the ionization conditions, Analytica Chimica Acta 2002; 461: 97-108 https://doi.org/10.1016/S0003-2670(02)00225-8
  8. Margalho C, de Boer D, Gallardo E, Barroso M and Vieira DN. Determination of furosemide in whole blood using SPE and GC-EI-MS, J Anal Toxicol 2005; 29(5): 309-313 https://doi.org/10.1093/jat/29.5.309
  9. Mutavdzic D, Horvat AJ, Babic S and Kastelan-Macan M. SPE-microwave-assisted extraction coupled system for the extraction of pesticides from water samples, J Sep Sci 2005; 28(13): 1485-1492 https://doi.org/10.1002/jssc.200400061
  10. Sharma VK, Jadhav RK, Rao GJ, Saraf AK and Chandra H. High performance liquid chromatographic method for the analysis of organophosphorus and carbamate pesticides, Forensic Sci Int 1990; 48(1): 21-25 https://doi.org/10.1016/0379-0738(90)90268-4
  11. Walles M, Mullett WM and Pawliszyn J. Monitoring of drugs and metabolites in whole blood by restricted-access solid-phase microextraction coupled to liquid chromatography-mass spectrometry, J Chromatogr A 2004; 30: 85-92 https://doi.org/10.1016/j.chroma.2003.08.068
  12. Zhu X, Yang J, Su Q, Cui J and Gao Y. Selective solid-phase extraction using molecularly imprinted polymer for the analysis of polar organophosphorus pesticides in water and soil samples, J Chromatogr A 2005; 1092(2): 161-169 https://doi.org/10.1016/j.chroma.2005.07.037