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Simultaneous derivatization and extraction of amphetamine and methylenedioxyamphetamine in urine with headspace liquid-phase microextraction followed by gas chromatography-mass spectrometry.
J Chromatogr A. 2008 Mar 21; 1185(1):19-22.JC

Abstract

A new method is reported for the simultaneous extraction and derivatization of amphetamine (AM) and methylenedioxyamphetamine (MDA) using headspace hollow fiber protected liquid-phase microextraction (HS-HF-LPME); quantitation is by gas chromatograph-mass spectrometry in the selected ion monitoring (SIM) mode. The derivatizing reagent, pentafluorobenzaldehyde (PFBAY), was added to the extraction solvent. The analytes, volatile and basic, were released from the sample matrix into the headspace first, then extracted and derivatized in the solvent. After that, 2 microl of extract was directly injected into the GC-MS system. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the concentration range investigated (50-350 ng ml(-1) for AM and 50-700 ng ml(-1) for MDA). Excellent repeatability of the extraction (RSD< or = 4%, n=5), and low limits of quantitation (0.25 ng ml(-1) for AM and 1.00 ng ml(-1) for MDA) were achieved. The feasibility of the method was demonstrated by analyzing human urine samples.

Authors+Show Affiliations

Department of Chemistry, National Tsing Hua University, Hsinchu, Taiwan.No affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

18258242

Citation

Chiang, Jing-Shan, and Shang-Da Huang. "Simultaneous Derivatization and Extraction of Amphetamine and Methylenedioxyamphetamine in Urine With Headspace Liquid-phase Microextraction Followed By Gas Chromatography-mass Spectrometry." Journal of Chromatography. A, vol. 1185, no. 1, 2008, pp. 19-22.
Chiang JS, Huang SD. Simultaneous derivatization and extraction of amphetamine and methylenedioxyamphetamine in urine with headspace liquid-phase microextraction followed by gas chromatography-mass spectrometry. J Chromatogr A. 2008;1185(1):19-22.
Chiang, J. S., & Huang, S. D. (2008). Simultaneous derivatization and extraction of amphetamine and methylenedioxyamphetamine in urine with headspace liquid-phase microextraction followed by gas chromatography-mass spectrometry. Journal of Chromatography. A, 1185(1), 19-22. https://doi.org/10.1016/j.chroma.2008.01.038
Chiang JS, Huang SD. Simultaneous Derivatization and Extraction of Amphetamine and Methylenedioxyamphetamine in Urine With Headspace Liquid-phase Microextraction Followed By Gas Chromatography-mass Spectrometry. J Chromatogr A. 2008 Mar 21;1185(1):19-22. PubMed PMID: 18258242.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simultaneous derivatization and extraction of amphetamine and methylenedioxyamphetamine in urine with headspace liquid-phase microextraction followed by gas chromatography-mass spectrometry. AU - Chiang,Jing-Shan, AU - Huang,Shang-Da, Y1 - 2008/01/20/ PY - 2007/12/07/received PY - 2008/01/15/revised PY - 2008/01/17/accepted PY - 2008/2/9/pubmed PY - 2008/5/3/medline PY - 2008/2/9/entrez SP - 19 EP - 22 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1185 IS - 1 N2 - A new method is reported for the simultaneous extraction and derivatization of amphetamine (AM) and methylenedioxyamphetamine (MDA) using headspace hollow fiber protected liquid-phase microextraction (HS-HF-LPME); quantitation is by gas chromatograph-mass spectrometry in the selected ion monitoring (SIM) mode. The derivatizing reagent, pentafluorobenzaldehyde (PFBAY), was added to the extraction solvent. The analytes, volatile and basic, were released from the sample matrix into the headspace first, then extracted and derivatized in the solvent. After that, 2 microl of extract was directly injected into the GC-MS system. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the concentration range investigated (50-350 ng ml(-1) for AM and 50-700 ng ml(-1) for MDA). Excellent repeatability of the extraction (RSD< or = 4%, n=5), and low limits of quantitation (0.25 ng ml(-1) for AM and 1.00 ng ml(-1) for MDA) were achieved. The feasibility of the method was demonstrated by analyzing human urine samples. SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/18258242/Simultaneous_derivatization_and_extraction_of_amphetamine_and_methylenedioxyamphetamine_in_urine_with_headspace_liquid_phase_microextraction_followed_by_gas_chromatography_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(08)00126-X DB - PRIME DP - Unbound Medicine ER -