title: Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride.
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 microgram/mL. The within run and between run precisions were higher (9.4% and 10.8%) at a urinary phenmetrazine concentration of 1.0 microgram/mL, which was very close to the detection limit of the assay. The assay was linear for urinary phenmetrazine concentration of 1 to 100 micrograms/mL with a detection limit of 0.5 microgram/mL.
authors.affiliation: Clinical Chemistry and Toxicology Laboratories, Albuquerque, NM, USA.
authors.forename: A
authors.initials: A
authors.lastname: Dasgupta
authors.forename: C E
authors.initials: CE
authors.lastname: Mahle
mesh_terms: D000662:Amphetamines / Q000652:urine; D002210:Caprylates / Q000737:chemistry*; D062787:Drug Overdose / Q000175:diagnosis; D017248:Enzyme Multiplied Immunoassay Technique; D005466:Fluorocarbons / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006801:Humans; D008970:Molecular Weight; D010633:Phenmetrazine / Q000737:chemistry / Q000506:poisoning / Q000652:urine*; D019966:Substance-Related Disorders / Q000175:diagnosis
chemical_list: D000662:Amphetamines; D002210:Caprylates; D005466:Fluorocarbons; C023036:perfluorooctanoic acid; D010633:Phenmetrazine