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Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride.
J Forensic Sci. 1997 Sep; 42(5):937-41.JF

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+Show Affiliations

Clinical Chemistry and Toxicology Laboratories, Albuquerque, NM, USA.No affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

9304848

Citation

Dasgupta, A, and C E. Mahle. "Determination of Phenmetrazine in Urine By Gas Chromatography-mass Spectrometry After Liquid-liquid Extraction and Derivatization With Perfluorooctanoyl Chloride." Journal of Forensic Sciences, vol. 42, no. 5, 1997, pp. 937-41.
Dasgupta A, Mahle CE. Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride. J Forensic Sci. 1997;42(5):937-41.
Dasgupta, A., & Mahle, C. E. (1997). Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride. Journal of Forensic Sciences, 42(5), 937-41.
Dasgupta A, Mahle CE. Determination of Phenmetrazine in Urine By Gas Chromatography-mass Spectrometry After Liquid-liquid Extraction and Derivatization With Perfluorooctanoyl Chloride. J Forensic Sci. 1997;42(5):937-41. PubMed PMID: 9304848.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Determination of phenmetrazine in urine by gas chromatography-mass spectrometry after liquid-liquid extraction and derivatization with perfluorooctanoyl chloride. AU - Dasgupta,A, AU - Mahle,C E, PY - 1997/9/26/pubmed PY - 1997/9/26/medline PY - 1997/9/26/entrez SP - 937 EP - 41 JF - Journal of forensic sciences JO - J. Forensic Sci. VL - 42 IS - 5 N2 - 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. SN - 0022-1198 UR - https://www.unboundmedicine.com/medline/citation/9304848/Determination_of_phenmetrazine_in_urine_by_gas_chromatography_mass_spectrometry_after_liquid_liquid_extraction_and_derivatization_with_perfluorooctanoyl_chloride_ DB - PRIME DP - Unbound Medicine ER -