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Simple and simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood by gas chromatography-mass spectrometry after headspace-solid phase microextraction and derivatization.
Forensic Sci Int. 2000 Apr 10; 109(3):215-23.FS

Abstract

A simple and sensitive method for the simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood was developed using a headspace-solid phase microextraction (SPME) and derivatization. A 0.5 g whole blood sample, 5 microl d(5)-methamphetamine (50 micrig/ml) as an internal standard, and 0.5 ml sodium hydroxide (1 M) were placed into a 12 ml vial, and sealed rapidly with a silicone septum and an aluminum cap. Immediately after the vial was heated to 70 degrees C in an aluminium block heater, the needle of the SPME device was inserted through the septum of the vial, and the extraction fiber was exposed in the headspace for 15 min. First, heptafluorobutyric anhydride was injected into the injection port of the GC-MS, and the compounds extracted by the fiber were then desorbed and derivatized simultaneously by exposing the fiber in the injection port. The calibration curves, using an internal standard method, demonstrated good linearity throughout the concentration range from 0.01 to 1.0 microg/g. The detection limits of this method were 5.0 ng/g for fenfluramine and methamphetamine, and 10 ng/g for amphetamine. No interferences were found, and the time for analysis was about 30 min for one sample. This method was applied to a suicide case in which the victim ingested fenfluramine. Fenfluramine was detected in the blood sample collected from the victim at the concentration of 7.7 microg/g.

Authors+Show Affiliations

Department of Legal Medicine, Hiroshima University School of Medicine, 1-2-3 Kasumi, Minami-ku, Hiroshima, Japan. namera@ipc.hiroshima-u.ac.jpNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Case Reports
Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

10725657

Citation

Namera, A, et al. "Simple and Simultaneous Analysis of Fenfluramine, Amphetamine and Methamphetamine in Whole Blood By Gas Chromatography-mass Spectrometry After Headspace-solid Phase Microextraction and Derivatization." Forensic Science International, vol. 109, no. 3, 2000, pp. 215-23.
Namera A, Yashiki M, Liu J, et al. Simple and simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood by gas chromatography-mass spectrometry after headspace-solid phase microextraction and derivatization. Forensic Sci Int. 2000;109(3):215-23.
Namera, A., Yashiki, M., Liu, J., Okajima, K., Hara, K., Imamura, T., & Kojima, T. (2000). Simple and simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood by gas chromatography-mass spectrometry after headspace-solid phase microextraction and derivatization. Forensic Science International, 109(3), 215-23.
Namera A, et al. Simple and Simultaneous Analysis of Fenfluramine, Amphetamine and Methamphetamine in Whole Blood By Gas Chromatography-mass Spectrometry After Headspace-solid Phase Microextraction and Derivatization. Forensic Sci Int. 2000 Apr 10;109(3):215-23. PubMed PMID: 10725657.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Simple and simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood by gas chromatography-mass spectrometry after headspace-solid phase microextraction and derivatization. AU - Namera,A, AU - Yashiki,M, AU - Liu,J, AU - Okajima,K, AU - Hara,K, AU - Imamura,T, AU - Kojima,T, PY - 2000/3/22/pubmed PY - 2000/6/8/medline PY - 2000/3/22/entrez SP - 215 EP - 23 JF - Forensic science international JO - Forensic Sci. Int. VL - 109 IS - 3 N2 - A simple and sensitive method for the simultaneous analysis of fenfluramine, amphetamine and methamphetamine in whole blood was developed using a headspace-solid phase microextraction (SPME) and derivatization. A 0.5 g whole blood sample, 5 microl d(5)-methamphetamine (50 micrig/ml) as an internal standard, and 0.5 ml sodium hydroxide (1 M) were placed into a 12 ml vial, and sealed rapidly with a silicone septum and an aluminum cap. Immediately after the vial was heated to 70 degrees C in an aluminium block heater, the needle of the SPME device was inserted through the septum of the vial, and the extraction fiber was exposed in the headspace for 15 min. First, heptafluorobutyric anhydride was injected into the injection port of the GC-MS, and the compounds extracted by the fiber were then desorbed and derivatized simultaneously by exposing the fiber in the injection port. The calibration curves, using an internal standard method, demonstrated good linearity throughout the concentration range from 0.01 to 1.0 microg/g. The detection limits of this method were 5.0 ng/g for fenfluramine and methamphetamine, and 10 ng/g for amphetamine. No interferences were found, and the time for analysis was about 30 min for one sample. This method was applied to a suicide case in which the victim ingested fenfluramine. Fenfluramine was detected in the blood sample collected from the victim at the concentration of 7.7 microg/g. SN - 0379-0738 UR - https://www.unboundmedicine.com/medline/citation/10725657/Simple_and_simultaneous_analysis_of_fenfluramine_amphetamine_and_methamphetamine_in_whole_blood_by_gas_chromatography_mass_spectrometry_after_headspace_solid_phase_microextraction_and_derivatization_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379073800001456 DB - PRIME DP - Unbound Medicine ER -