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Gas chromatography-electron ionization and chemical ionization mass spectrometric analysis of urinary phenmetrazine after derivatization with 4-carbethoxyhexafluorobutyryl chloride--a new derivative.
J Forensic Sci. 1998 May; 43(3):636-40.JF

Abstract

Phenmetrazine is a central nervous system stimulant currently used as an anorectic agent. The drug is abused and is reported to cause death from overdose. We describe a new derivatization method for phenmetrazine using 4-carbethoxyhexafluorobutyryl chloride. Quantitation of urinary phenmetrazine can be easily achieved by using N-ethyl amphetamine as an internal standard. The electron ionization mass spectrum of 4-carbethoxyhexafluorobutyryl derivative of phenmetrazine showed a molecular ion at m/z 427 and a base peak at m/z 70. In the methane chemical ionization mass spectrum, the base peak was observed at m/z 428 (protonated molecular ion). In the electron ionization mass spectrum of 4-carbethoxyhexafluorobutyryl derivative of the internal standard, N-ethyl amphetamine we did not observe a molecular ion. However, in the chemical ionization mass spectrum, the protonated molecular ion at m/z 414 was the base peak. The retention time of derivatized phenmetrazine (8.4 min) was substantially longer than the retention time of the underivatized molecule. Moreover, underivatized phenmetrazine showed poor peak shape (substantial tailing) while derivatized phenmetrazine had excellent chromatographic properties. The within-run and between-run precisions of the assay were 2.6% and 3.1% respectively at a urinary phenmetrazine concentration of 10 micrograms/mL. The assay was linear for urinary phenmetrazine concentration of 1 to 100 micrograms/mL with a detection limit of 0.2 microgram/mL.

Authors+Show Affiliations

Pathology and Laboratory Medicine, University of Texas-Houston Medical School, Houston, USA.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

9608702

Citation

Dasgupta, A, et al. "Gas Chromatography-electron Ionization and Chemical Ionization Mass Spectrometric Analysis of Urinary Phenmetrazine After Derivatization With 4-carbethoxyhexafluorobutyryl Chloride--a New Derivative." Journal of Forensic Sciences, vol. 43, no. 3, 1998, pp. 636-40.
Dasgupta A, Hart A, Humphrey P, et al. Gas chromatography-electron ionization and chemical ionization mass spectrometric analysis of urinary phenmetrazine after derivatization with 4-carbethoxyhexafluorobutyryl chloride--a new derivative. J Forensic Sci. 1998;43(3):636-40.
Dasgupta, A., Hart, A., Humphrey, P., & Blackwell, W. (1998). Gas chromatography-electron ionization and chemical ionization mass spectrometric analysis of urinary phenmetrazine after derivatization with 4-carbethoxyhexafluorobutyryl chloride--a new derivative. Journal of Forensic Sciences, 43(3), 636-40.
Dasgupta A, et al. Gas Chromatography-electron Ionization and Chemical Ionization Mass Spectrometric Analysis of Urinary Phenmetrazine After Derivatization With 4-carbethoxyhexafluorobutyryl Chloride--a New Derivative. J Forensic Sci. 1998;43(3):636-40. PubMed PMID: 9608702.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Gas chromatography-electron ionization and chemical ionization mass spectrometric analysis of urinary phenmetrazine after derivatization with 4-carbethoxyhexafluorobutyryl chloride--a new derivative. AU - Dasgupta,A, AU - Hart,A, AU - Humphrey,P, AU - Blackwell,W, PY - 1998/6/3/pubmed PY - 1998/6/3/medline PY - 1998/6/3/entrez SP - 636 EP - 40 JF - Journal of forensic sciences JO - J. Forensic Sci. VL - 43 IS - 3 N2 - Phenmetrazine is a central nervous system stimulant currently used as an anorectic agent. The drug is abused and is reported to cause death from overdose. We describe a new derivatization method for phenmetrazine using 4-carbethoxyhexafluorobutyryl chloride. Quantitation of urinary phenmetrazine can be easily achieved by using N-ethyl amphetamine as an internal standard. The electron ionization mass spectrum of 4-carbethoxyhexafluorobutyryl derivative of phenmetrazine showed a molecular ion at m/z 427 and a base peak at m/z 70. In the methane chemical ionization mass spectrum, the base peak was observed at m/z 428 (protonated molecular ion). In the electron ionization mass spectrum of 4-carbethoxyhexafluorobutyryl derivative of the internal standard, N-ethyl amphetamine we did not observe a molecular ion. However, in the chemical ionization mass spectrum, the protonated molecular ion at m/z 414 was the base peak. The retention time of derivatized phenmetrazine (8.4 min) was substantially longer than the retention time of the underivatized molecule. Moreover, underivatized phenmetrazine showed poor peak shape (substantial tailing) while derivatized phenmetrazine had excellent chromatographic properties. The within-run and between-run precisions of the assay were 2.6% and 3.1% respectively at a urinary phenmetrazine concentration of 10 micrograms/mL. The assay was linear for urinary phenmetrazine concentration of 1 to 100 micrograms/mL with a detection limit of 0.2 microgram/mL. SN - 0022-1198 UR - https://www.unboundmedicine.com/medline/citation/9608702/Gas_chromatography_electron_ionization_and_chemical_ionization_mass_spectrometric_analysis_of_urinary_phenmetrazine_after_derivatization_with_4_carbethoxyhexafluorobutyryl_chloride__a_new_derivative_ DB - PRIME DP - Unbound Medicine ER -