Tags

Type your tag names separated by a space and hit enter

A convenient derivatization method for gas chromatography/mass spectrometric determination of phenmetrazine in urine using 2,2,2-trichloroethyl chloroformate.
J Forensic Sci. 1998 May; 43(3):630-5.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 2,2,2-trichloroethyl chloroformate. Quantitation of urinary phenmetrazine can be easily achieved by using N-propylamphetamine as an internal standard. The phenmetrazine 2,2,2-trichloroethyl carbamate showed a molecular ion isotope cluster at m/z 351, 353, 355, and 357 (isotope effect of three chlorine atoms in the derivatized molecule) and other peaks at m/z 247, 245, 204, 114, and 70 in the electron ionization mass spectrometry, thus aiding in unambiguous identification. The underivatized phenmetrazine showed a relatively weaker molecular ion at m/z 177 and a base peak at m/z 71. The N-propylamphetamine 2,2,2-trichloroethyl carbamate (internal standard) showed a very weak molecular ion at m/z 351 and a base peak at m/z 260. Another strong characteristic peak at m/z 91 was also observed. The retention time of derivatized phenmetrazine (9.5 min) was substantially longer than the retention time of the underivatized molecule (2.5 min). Moreover, underivatized phenmetrazine showed poor peak shape (substantial tailing) while derivatized phenmetrazine had excellent chromatographic property. The within-run and between-run precisions of the assay were 1.9% and 3.2% at a urinary phenmetrazine concentration of 20 micrograms/mL. The assay was linear for urinary phenmetrazine concentration of 1 microgram/mL to 100 micrograms/mL with a detection limit of 0.5 microgram/mL.

Authors+Show Affiliations

Clinical Chemistry and Toxicology Laboratory, University of New Mexico Health Sciences Center, Albuquerque, USA.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

9608701

Citation

Dasgupta, A, et al. "A Convenient Derivatization Method for Gas Chromatography/mass Spectrometric Determination of Phenmetrazine in Urine Using 2,2,2-trichloroethyl Chloroformate." Journal of Forensic Sciences, vol. 43, no. 3, 1998, pp. 630-5.
Dasgupta A, Handler MS, Nine JS. A convenient derivatization method for gas chromatography/mass spectrometric determination of phenmetrazine in urine using 2,2,2-trichloroethyl chloroformate. J Forensic Sci. 1998;43(3):630-5.
Dasgupta, A., Handler, M. S., & Nine, J. S. (1998). A convenient derivatization method for gas chromatography/mass spectrometric determination of phenmetrazine in urine using 2,2,2-trichloroethyl chloroformate. Journal of Forensic Sciences, 43(3), 630-5.
Dasgupta A, Handler MS, Nine JS. A Convenient Derivatization Method for Gas Chromatography/mass Spectrometric Determination of Phenmetrazine in Urine Using 2,2,2-trichloroethyl Chloroformate. J Forensic Sci. 1998;43(3):630-5. PubMed PMID: 9608701.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A convenient derivatization method for gas chromatography/mass spectrometric determination of phenmetrazine in urine using 2,2,2-trichloroethyl chloroformate. AU - Dasgupta,A, AU - Handler,M S, AU - Nine,J S, PY - 1998/6/3/pubmed PY - 1998/6/3/medline PY - 1998/6/3/entrez SP - 630 EP - 5 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 2,2,2-trichloroethyl chloroformate. Quantitation of urinary phenmetrazine can be easily achieved by using N-propylamphetamine as an internal standard. The phenmetrazine 2,2,2-trichloroethyl carbamate showed a molecular ion isotope cluster at m/z 351, 353, 355, and 357 (isotope effect of three chlorine atoms in the derivatized molecule) and other peaks at m/z 247, 245, 204, 114, and 70 in the electron ionization mass spectrometry, thus aiding in unambiguous identification. The underivatized phenmetrazine showed a relatively weaker molecular ion at m/z 177 and a base peak at m/z 71. The N-propylamphetamine 2,2,2-trichloroethyl carbamate (internal standard) showed a very weak molecular ion at m/z 351 and a base peak at m/z 260. Another strong characteristic peak at m/z 91 was also observed. The retention time of derivatized phenmetrazine (9.5 min) was substantially longer than the retention time of the underivatized molecule (2.5 min). Moreover, underivatized phenmetrazine showed poor peak shape (substantial tailing) while derivatized phenmetrazine had excellent chromatographic property. The within-run and between-run precisions of the assay were 1.9% and 3.2% at a urinary phenmetrazine concentration of 20 micrograms/mL. The assay was linear for urinary phenmetrazine concentration of 1 microgram/mL to 100 micrograms/mL with a detection limit of 0.5 microgram/mL. SN - 0022-1198 UR - https://www.unboundmedicine.com/medline/citation/9608701/A_convenient_derivatization_method_for_gas_chromatography/mass_spectrometric_determination_of_phenmetrazine_in_urine_using_222_trichloroethyl_chloroformate_ DB - PRIME DP - Unbound Medicine ER -