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Development of a harmonised method for the profiling of amphetamines: IV. Optimisation of sample preparation
Authors:Andersson Kjell  Jalava Kaisa  Lock Eric  Huizer Henk  Kaa Elisabet  Lopes Alvaro  Poortman-van der Meer Anneke  Cole Michael D  Dahlén Johan  Sippola Erkki
Institution:1. Swedish National Laboratory of Forensic Science-SKL, SE-581 94 Linköping, Sweden;2. National Bureau of Investigation, P.O. Box 285, FIN-01301 Vantaa, Finland;3. Institut de Police Scientifique, University of Lausanne, Batiment de Chimie, CH-1015 Lausanne-Dorigny, Switzerland;4. Netherlands Forensic Institute, Postbus 24044, 2490AA Den Haag, The Netherlands;5. Department of Forensic Medicine, University of Aarhus, Skovagervej 2, DK-8240 Risskov, Denmark;6. Laboratorio de Policia Cientifica, Policia Judiciaria, Rua Gomes Freire 174, 1169-007 Lisbon, Portugal;g Forensic Science Unit, University of Strathclyde, 204 George Street, Glasgow G1 1XW, United Kingdom
Abstract:The suitability of liquid-liquid extraction (LLE) and solid-phase extraction (SPE) for the preparation of impurity extracts intended for gas chromatographic profiling analyses of amphetamine were evaluated. Both techniques were optimised with respect to the extraction of selected target compounds by use of full factorial designs in which the variables affecting the performance were evaluated. Test samples consisted of amphetamine synthesised by the Leuckart reaction, by reductive amination of benzyl methyl ketone and by the nitrostyrene route. The performance of LLE and SPE were comparable in terms of repeatability and recovery of the target compounds. LLE was considered the better choice for the present harmonised amphetamine profiling method due to the lack of information on the long-term stability of SPE columns.
Keywords:Amphetamine  Impurities  Profiling  Optimisation  SPE  LLE  GC-FID  GC–MS
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