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Gas chromatography/mass spectrometry determination of amphetamine-related drugs and ephedrines in plasma, urine and hair samples after derivatization with 2,2,2-trichloroethyl chloroformate.
Rapid Commun Mass Spectrom. 2005; 19(7):919-27.RC

Abstract

A new analytical approach, based on derivatization with 2,2,2-trichloroethyl chloroformate and gas chromatography/mass spectrometry (GC/MS), was investigated for qualitative and quantitative analyses of a large range of amphetamine-related drugs and ephedrines in plasma, urine and hair samples. Sample preparation involved alkaline extraction of analytes from biological samples using Extrelut columns, after addition of the internal standard 3,4-methylenedioxypropylamphetamine (MDPA), and subsequent derivatization to produce 2,2,2-trichloroethylcarbamates. GC/MS analyses, in splitless mode using a slightly polar 30-m capillary column, were performed with quadrupole or ion trap instruments. MS acquisition modes were electron ionization (EI) in full-scan or selected ion monitoring (SIM) modes (quadrupole), and full-scan MS or MS/MS modes with chemical ionization (CI) conditions (ion trap). EI spectra of 2,2,2-trichloroethylcarbamates showed variably abundant molecular ions as well as abundant diagnostic fragment ions, both characterized by ion clusters reflecting the isotope distribution of three chlorine atoms in the derivatized molecules. CI spectra showed abundant protonated molecules. Quantitative studies using EI SIM conditions gave recoveries in the range 74-89%, linear response over ranges of 10-2000 ng/mL (plasma and urine) and 0.20-20 ng/mg (hair), with corresponding limits of detection in the ranges 2-5 ng/mL and 0.1-0.2 ng/mg. Potential applications (following full method validation) include clinical and forensic toxicology, as well as doping control.

Authors+Show Affiliations

Forensic Toxicology and Antidoping, University Hospital of Padova, Via Falloppio 50, I-35121 Padova, Italy.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

15747332

Citation

Frison, Giampietro, et al. "Gas Chromatography/mass Spectrometry Determination of Amphetamine-related Drugs and Ephedrines in Plasma, Urine and Hair Samples After Derivatization With 2,2,2-trichloroethyl Chloroformate." Rapid Communications in Mass Spectrometry : RCM, vol. 19, no. 7, 2005, pp. 919-27.
Frison G, Tedeschi L, Favretto D, et al. Gas chromatography/mass spectrometry determination of amphetamine-related drugs and ephedrines in plasma, urine and hair samples after derivatization with 2,2,2-trichloroethyl chloroformate. Rapid Commun Mass Spectrom. 2005;19(7):919-27.
Frison, G., Tedeschi, L., Favretto, D., Reheman, A., & Ferrara, S. D. (2005). Gas chromatography/mass spectrometry determination of amphetamine-related drugs and ephedrines in plasma, urine and hair samples after derivatization with 2,2,2-trichloroethyl chloroformate. Rapid Communications in Mass Spectrometry : RCM, 19(7), 919-27.
Frison G, et al. Gas Chromatography/mass Spectrometry Determination of Amphetamine-related Drugs and Ephedrines in Plasma, Urine and Hair Samples After Derivatization With 2,2,2-trichloroethyl Chloroformate. Rapid Commun Mass Spectrom. 2005;19(7):919-27. PubMed PMID: 15747332.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Gas chromatography/mass spectrometry determination of amphetamine-related drugs and ephedrines in plasma, urine and hair samples after derivatization with 2,2,2-trichloroethyl chloroformate. AU - Frison,Giampietro, AU - Tedeschi,Luciano, AU - Favretto,Donata, AU - Reheman,Aikebaier, AU - Ferrara,Santo Davide, PY - 2005/3/5/pubmed PY - 2005/5/12/medline PY - 2005/3/5/entrez SP - 919 EP - 27 JF - Rapid communications in mass spectrometry : RCM JO - Rapid Commun Mass Spectrom VL - 19 IS - 7 N2 - A new analytical approach, based on derivatization with 2,2,2-trichloroethyl chloroformate and gas chromatography/mass spectrometry (GC/MS), was investigated for qualitative and quantitative analyses of a large range of amphetamine-related drugs and ephedrines in plasma, urine and hair samples. Sample preparation involved alkaline extraction of analytes from biological samples using Extrelut columns, after addition of the internal standard 3,4-methylenedioxypropylamphetamine (MDPA), and subsequent derivatization to produce 2,2,2-trichloroethylcarbamates. GC/MS analyses, in splitless mode using a slightly polar 30-m capillary column, were performed with quadrupole or ion trap instruments. MS acquisition modes were electron ionization (EI) in full-scan or selected ion monitoring (SIM) modes (quadrupole), and full-scan MS or MS/MS modes with chemical ionization (CI) conditions (ion trap). EI spectra of 2,2,2-trichloroethylcarbamates showed variably abundant molecular ions as well as abundant diagnostic fragment ions, both characterized by ion clusters reflecting the isotope distribution of three chlorine atoms in the derivatized molecules. CI spectra showed abundant protonated molecules. Quantitative studies using EI SIM conditions gave recoveries in the range 74-89%, linear response over ranges of 10-2000 ng/mL (plasma and urine) and 0.20-20 ng/mg (hair), with corresponding limits of detection in the ranges 2-5 ng/mL and 0.1-0.2 ng/mg. Potential applications (following full method validation) include clinical and forensic toxicology, as well as doping control. SN - 0951-4198 UR - https://www.unboundmedicine.com/medline/citation/15747332/Gas_chromatography/mass_spectrometry_determination_of_amphetamine_related_drugs_and_ephedrines_in_plasma_urine_and_hair_samples_after_derivatization_with_222_trichloroethyl_chloroformate_ L2 - https://doi.org/10.1002/rcm.1873 DB - PRIME DP - Unbound Medicine ER -