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Analysis of amphetamine, methamphetamine, methylenedioxyamphetamine and methylenedioxymethamphetamine in whole blood using in-matrix ethyl chloroformate derivatization and automated headspace solid-phase microextraction followed by GC-MS

Forensic Toxicology volume 26, pages 66–70 (2008)Cite this article

Abstract

The in-matrix alkyl chloroformate derivatization method for amphetamine, methamphetamine, methylenedioxyamphetamine (MDA), and methylene-dioxymethamphetamine (MDMA) was adapted for use with the whole blood matrix. This derivatization method was followed by automated headspace (HS)-solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) analysis. The sensitivity of this method, expressed as limit of detection, was approximately 10 ng/ml for these analytes tested in the blood matrix, which was sufficient to detect toxic concentrations of amphetamines in blood. The limit of quantitation for target analytes ranged from 0.05 to 0.2 μg/ml. The intraday precision and accuracy studies generally showed satisfactory results for all target compounds except MDA, in which a larger variation was observed. The in-matrix ethyl chloroformate derivatization of amphetamine, methamphetamine, MDA, and MDMA for HS-SPME was tested in other matrices such as stomach fluid, bile, thoracic cavity fluid, vitreous humor, brain, liver, spleen, and skeletal muscle. As a result, stomach fluid, thoracic cavity fluid, and vitreous humor showed SPME efficiencies higher than that of whole blood; however, this method was not suitable for solid tissue matrices under the present conditions.

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References

  1. Pawliszyn J, Arthur C (1990) Solid phase microextraction with thermal desorption using fused silica optical fibers. Anal Chem 62:2145–2148

    Article  Google Scholar 

  2. Zhang Z, Pawliszyn J (1993) Headspace solid-phase microextraction. Anal Chem 65:1843–1852

    Article  CAS  Google Scholar 

  3. Mills GA, Walker V (2000) Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials. J Chromatogr A 902:267–287

    Article  PubMed  CAS  Google Scholar 

  4. Namera A, Yashiki M, Kojima T, Ueki M (2002) Automated headspace solid-phase microextraction and in-matrix derivatization for the determination of amphetamine-related drugs in human urine by gas chromatography-mass spectrometry. J Chromatogr Sci 40:19–25

    PubMed  CAS  Google Scholar 

  5. Yashiki M, Kojima T, Miyazaki T, Nagasawa N, Iwasaki Y, Hara K (1995) Detection of amphetamines in urine using head space-solid phase microextraction and chemical ionization selected ion monitoring. Forensic Sci Int 76:169–177

    Article  PubMed  CAS  Google Scholar 

  6. Centini F, Masti A, Barni Comparini I (1996) Quantitative and qualitative analysis of MDMA, MDEA, MA and amphetamine in urine by headspace/solid phase micro-extraction (SPME) and GC/MS. Forensic Sci Int 83:161–166

    Article  PubMed  CAS  Google Scholar 

  7. Battu C, Marquet P, Fauconnet AL, Lacassie E, Lachatre G (1998) Screening procedure for 21 amphetamine-related compounds in urine using solid-phase microextraction and gas chromatography-mass spectrometry. J Chromatogr Sci 36: 1–7

    PubMed  CAS  Google Scholar 

  8. Jurado C, Gimenez MP, Soriano T, Menendez M, Repetto M (2000) Rapid analysis of amphetamine, methamphetamine, MDA, and MDMA in urine using solid-phase microextraction, direct on-fiber derivatization, and analysis by GC-MS. J Anal Toxicol 24:11–16

    PubMed  CAS  Google Scholar 

  9. Nagasawa N, Yashiki M, Iwasaki Y, Hara K, Kojima T (1996) Rapid analysis of amphetamines in blood using head space-solid phase microextraction and selected ion monitoring. Forensic Sci Int 78:95–102

    Article  PubMed  CAS  Google Scholar 

  10. Namera A, Yashiki M, Liu J, Okajima K, Hara K, Imamura T, Kojima T (2000) Simple and simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood by gas chromatography-mass spectrometry after headspace-solid phase microextraction and derivatization. Forensic Sci Int 109:215–223

    Article  PubMed  CAS  Google Scholar 

  11. Okajima K, Namera A, Yashiki M, Tsukue I, Kojima T (2001) Highly sensitive analysis of methamphetamine and amphetamine in human whole blood using headspace solid-phase microextraction and gas chromatography-mass spectrometry. Forensic Sci Int 116:15–22

    Article  PubMed  CAS  Google Scholar 

  12. Koide I, Noguchi O, Okada K, Yokoyama A, Oda H, Yamamoto S, Kataoka H (1998) Determination of amphetamine and methamphetamine in human hair by headspace solid-phase microextraction and gas chromatography with nitrogen-phosphorus detection. J Chromatogr B 707:99–104

    Article  CAS  Google Scholar 

  13. Sporkert F, Pragst F (2000) Use of headspace solid-phase microextraction (HS-SPME) in hair analysis for organic compounds. Forensic Sci Int 107:129–148

    Article  PubMed  CAS  Google Scholar 

  14. Liu J, Hara K, Kashimura S, Kashiwagi M, Kageura M (2001) New method of derivatization and headspace solidphase microextraction for gas chromatographic-mass spectrometric analysis of amphetamines in hair. J Chromatogr B 758:95–101

    Article  CAS  Google Scholar 

  15. Raikos N, Christopoulou K, Theodoridis G, Tsoukali H, Psaroulis D (2003) Determination of amphetamines in human urine by headspace solid-phase microextraction and gas chromatography. J Chromatogr B 789:59–63

    Article  CAS  Google Scholar 

  16. Sato M, Mitsui T (1997) Rapid and simple determination of methamphetamine and amphetamine in blood by simultaneous extraction-derivatization. J Pharm Biomed Anal 16: 139–145

    Article  PubMed  CAS  Google Scholar 

  17. Pawliszyn J (2001) Solid phase microextraction. Adv Exp Med Biol 488:73–87

    PubMed  CAS  Google Scholar 

  18. Schulz M, Schmoldt A (2003) Therapeutic and toxic blood concentrations of more than 800 drugs and other xenobiotics. Pharmazie 58:447–474

    PubMed  CAS  Google Scholar 

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Authors and Affiliations

  1. Harris County Medical Examiner Office, Houston, Texas, USA

    Jeff Wise, Terry Danielson & Ashraf Mozayani

  2. Department of Science, John Jay College of Criminal Justice, The City University of New York, 445 West 59th Street, New York, NY, 10019, USA

    Richard Li

Authors
  1. Jeff Wise
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  2. Terry Danielson
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  3. Ashraf Mozayani
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  4. Richard Li
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Correspondence to Richard Li.

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Wise, J., Danielson, T., Mozayani, A. et al. Analysis of amphetamine, methamphetamine, methylenedioxyamphetamine and methylenedioxymethamphetamine in whole blood using in-matrix ethyl chloroformate derivatization and automated headspace solid-phase microextraction followed by GC-MS. Forensic Toxicol 26, 66–70 (2008). https://doi.org/10.1007/s11419-008-0048-8

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  • DOI: https://doi.org/10.1007/s11419-008-0048-8

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