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Automated headspace solid-phase microextraction and in-matrix derivatization for the determination of amphetamine-related drugs in human urine by gas chromatography-mass spectrometry.
J Chromatogr Sci. 2002 Jan; 40(1):19-25.JC

Abstract

An automated extraction and determination method for the gas chromatography (GC)-mass spectrometry (MS) analysis of amphetamine-related drugs in human urine is developed using headspace solid-phase microextraction (SPME) and in-matrix derivatization. A urine sample (0.5 mL, potassium carbonate (5 M, 1.0 mL), sodium chloride (0.5 g), and ethylchloroformate (20 microL) are put in a sample vial. Amphetamine-related drugs are converted to ethylformate derivatives (carbamates) in the vial because amphetamine-related drugs in urine are quickly reacted with ethylchloroformate. An SPME fiber is then exposed at 80 degrees C for 15 min in the headspace of the vial. The extracted derivatives to the fiber are desorbed by exposing the fiber in the injection port of a GC-MS. The calibration curves show linearity in the range of 1.0 to 1000 ng/mL for methamphetamine, fenfluramine, and methylenedioxymethamphetamine; 2.0 to 1000 ng/mL for amphetamine and phentermine; 5.0 to 1000 ng/mL for methylenedioxyamphetamine; 10 to 1000 ng/mL for phenethylamine; and 50 to 1000 ng/mL for 4-bromo-2,5-dimethoxyphenethylamine in urine. No interferences are found, and the time for analysis is 30 min for one sample. Furthermore, this proposed method is applied to some clinical and medico-legal cases by taking methamphetamine. Methamphetamine and its metabolite amphetamine are detected in the urine samples collected from the patients involved in the clinical cases. Methamphetamine, amphetamine, and phenethylamine are detected in the urine sample collected from the victim of a medico-legal case.

Authors+Show Affiliations

Department of Legal Medicine, Hiroshima University, Faculty of Medicine, Japan. namera@hiroshima-u.ac.jpNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

11866382

Citation

Namera, Akira, et al. "Automated Headspace Solid-phase Microextraction and In-matrix Derivatization for the Determination of Amphetamine-related Drugs in Human Urine By Gas Chromatography-mass Spectrometry." Journal of Chromatographic Science, vol. 40, no. 1, 2002, pp. 19-25.
Namera A, Yashiki M, Kojima T, et al. Automated headspace solid-phase microextraction and in-matrix derivatization for the determination of amphetamine-related drugs in human urine by gas chromatography-mass spectrometry. J Chromatogr Sci. 2002;40(1):19-25.
Namera, A., Yashiki, M., Kojima, T., & Ueki, M. (2002). Automated headspace solid-phase microextraction and in-matrix derivatization for the determination of amphetamine-related drugs in human urine by gas chromatography-mass spectrometry. Journal of Chromatographic Science, 40(1), 19-25.
Namera A, et al. Automated Headspace Solid-phase Microextraction and In-matrix Derivatization for the Determination of Amphetamine-related Drugs in Human Urine By Gas Chromatography-mass Spectrometry. J Chromatogr Sci. 2002;40(1):19-25. PubMed PMID: 11866382.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Automated headspace solid-phase microextraction and in-matrix derivatization for the determination of amphetamine-related drugs in human urine by gas chromatography-mass spectrometry. AU - Namera,Akira, AU - Yashiki,Mikio, AU - Kojima,Tohru, AU - Ueki,Makoto, PY - 2002/2/28/pubmed PY - 2002/3/20/medline PY - 2002/2/28/entrez SP - 19 EP - 25 JF - Journal of chromatographic science JO - J Chromatogr Sci VL - 40 IS - 1 N2 - An automated extraction and determination method for the gas chromatography (GC)-mass spectrometry (MS) analysis of amphetamine-related drugs in human urine is developed using headspace solid-phase microextraction (SPME) and in-matrix derivatization. A urine sample (0.5 mL, potassium carbonate (5 M, 1.0 mL), sodium chloride (0.5 g), and ethylchloroformate (20 microL) are put in a sample vial. Amphetamine-related drugs are converted to ethylformate derivatives (carbamates) in the vial because amphetamine-related drugs in urine are quickly reacted with ethylchloroformate. An SPME fiber is then exposed at 80 degrees C for 15 min in the headspace of the vial. The extracted derivatives to the fiber are desorbed by exposing the fiber in the injection port of a GC-MS. The calibration curves show linearity in the range of 1.0 to 1000 ng/mL for methamphetamine, fenfluramine, and methylenedioxymethamphetamine; 2.0 to 1000 ng/mL for amphetamine and phentermine; 5.0 to 1000 ng/mL for methylenedioxyamphetamine; 10 to 1000 ng/mL for phenethylamine; and 50 to 1000 ng/mL for 4-bromo-2,5-dimethoxyphenethylamine in urine. No interferences are found, and the time for analysis is 30 min for one sample. Furthermore, this proposed method is applied to some clinical and medico-legal cases by taking methamphetamine. Methamphetamine and its metabolite amphetamine are detected in the urine samples collected from the patients involved in the clinical cases. Methamphetamine, amphetamine, and phenethylamine are detected in the urine sample collected from the victim of a medico-legal case. SN - 0021-9665 UR - https://www.unboundmedicine.com/medline/citation/11866382/Automated_headspace_solid_phase_microextraction_and_in_matrix_derivatization_for_the_determination_of_amphetamine_related_drugs_in_human_urine_by_gas_chromatography_mass_spectrometry_ L2 - https://academic.oup.com/chromsci/article-lookup/doi/10.1093/chromsci/40.1.19 DB - PRIME DP - Unbound Medicine ER -