Volume 42, Issue 5 (September 1997)

    Determination of Phenmetrazine in Urine by Gas Chromatography-Mass Spectrometry after Liquid-Liquid Extraction and Derivatization with Perfluorooctanoyl Chloride

    (Received 2 December 1996; accepted 24 January 1997)

    CODEN: JFSOAD

      Format Pages Price  
    PDF Version 5 $25   ADD TO CART


    Abstract

    Phenmetrazine is a central nervous system stimulant and is currently used as an anorectic agent. The drug is abused and reported to cause death from overdose. We describe a liquid-liquid extraction protocol for phenmetrazine from urine using 1-chlorobutane and subsequent derivatization using perfluorooctanoyl chloride for gas chromatography-mass spectrometric confirmation. Quantitation of urinary phenmetrazine can be easily achieved by using N-propylamphetamine as an internal standard. The perfluorooctanoyl derivative of phenmetrazine showed a weak molecular ion at m/z 573 and a characteristic strong peak at m/z 467 in the electron ionization mass spectrometry thus aiding unambiguous identification. The perfluorooctanoyl derivative of the internal standard did not show any molecular ion, but showed strong characteristic peaks at m/z 482 and 440. The within run and between run precisions of the assay were 1.7% and 3.2% at a urinary phenmetrazine concentration of 20 µg/mL. The within run and between run precisions were higher (9.4% and 10.8%) at a urinary phenmetrazine concentration of 1.0 µg/mL, which was very close to the detection limit of the assay. The assay was linear for urinary phenmetrazine concentration of 1 to 100 µg/mL with a detection limit of 0.5 µg/mL.


    Author Information:

    Dasgupta, A
    Associate professor of pathology and director of the Clinical Chemistry and Toxicology Laboratories, Albuquerque, NM

    Mahle, CE
    resident physician, University of New Mexico Health Sciences Center, Albuquerque, NM


    Stock #: JFS14236J

    ISSN: 0022-1198

    DOI: 10.1520/JFS14236J

    ASTM International
    is a member of CrossRef.

    Author
    Title Determination of Phenmetrazine in Urine by Gas Chromatography-Mass Spectrometry after Liquid-Liquid Extraction and Derivatization with Perfluorooctanoyl Chloride
    Symposium , 0000-00-00
    Committee E30