Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride
Dasgupta, A
Associate professor of pathology and director of the Clinical Chemistryand Toxicology Laboratories, Albuquerque, NM.

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


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 l-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 mg/mL. The within run and between run precisions were higher (9.4% and 10.8%) at a urinary phenmetrazine concentration of 1.0 mg/mL, which was very close to the detection limit of the assay. The assay was linear for urinary phenmetrazine concentration of 1 to 100 mg/mL with a detection limit of 0.5 mg/mL.

Keywords:
forensic science, forensic toxicology phenmetrazine, gas chromatography/mass spectrometry, gas chromatography-mass spectrometry, perfluorooctanoyl, perfluorooctanoyl derivative, phenmetrazine, toxicology

Paper ID: JFS425970937

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Author Dasgupta A, Mahle CE Title Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride Symposium , Committee on