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Andersson K, Jalava K, Lock E, et al. Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method. Forensic Sci Int. 2006;169(1):50-63doi: 10.1016/j.forsciint.2006.10.018.
Andersson, K., Jalava, K., Lock, E., Finnon, Y., Huizer, H., Kaa, E., Lopes, A., Poortman-van der Meer, A., Cole, M. D., Dahlén, J., & Sippola, E. (2007). Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method. Forensic science international, 169(1), 50-63. https://doi.org/10.1016/j.forsciint.2006.10.018
Andersson, Kjell, et al. "Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method." Forensic science international vol. 169,1 (2007): 50-63. doi: https://doi.org/10.1016/j.forsciint.2006.10.018
Andersson K, Jalava K, Lock E, Finnon Y, Huizer H, Kaa E, Lopes A, Poortman-van der Meer A, Cole MD, Dahlén J, Sippola E. Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method. Forensic Sci Int. 2007 Jun 14;169(1):50-63. doi: 10.1016/j.forsciint.2006.10.018. Epub 2006 Dec 15. PMID: 17174497.
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Forensic Sci Int. 2007 Jun 14;169(1):50-63. doi: 10.1016/j.forsciint.2006.10.018. Epub 2006 Dec 15.

Development of a harmonised method for the profiling of amphetamines: III. Development of the gas chromatographic method.

Forensic science international

Kjell Andersson, Kaisa Jalava, Eric Lock, Yvonne Finnon, Henk Huizer, Elisabet Kaa, Alvaro Lopes, Anneke Poortman-van der Meer, Michael D Cole, Johan Dahlén, Erkki Sippola

Affiliations

  1. Swedish National Laboratory of Forensic Science-SKL, SE-581 94 Linköping, Sweden. [email protected]

PMID: 17174497 DOI: 10.1016/j.forsciint.2006.10.018

Abstract

This study focused on gas chromatographic analysis of target compounds found in illicit amphetamine synthesised by the Leuckart reaction, reductive amination of benzyl methyl ketone, and the nitrostyrene route. The analytical method was investigated and optimised with respect to introduction of amphetamine samples into the gas chromatograph and separation and detection of the target substances. Sample introduction using split and splitless injection was tested at different injector temperatures, and their ability to transfer the target compounds to the GC column was evaluated using cold on column injection as a reference. Taking the results from both techniques into consideration a temperature of 250 degrees C was considered to be the best compromise. The most efficient separation was achieved with a DB-35MS capillary column (35% diphenyl 65% dimethyl silicone; 30 m x 0.25 mm, d(f) 0.25 microm) and an oven temperature program that started at 90 degrees C (1 min) and was increased by 8 degrees C/min to 300 degrees C (10 min). Reproducibility, repeatability, linearity, and limits of determination for the flame ionisation detector (FID), nitrogen phosphorous detector (NPD), and mass spectrometry (MS) in scan mode and selected ion monitoring (SIM) mode were evaluated. In addition, selectivity was studied applying FID and MS in both scan and SIM mode. It was found that reproducibility, repeatability, and limits of determination were similar for FID, NPD, and MS in scan mode. Moreover, the linearity was better when applying FID or NPD whereas the selectivity was better when utilising the MS. Finally, the introduction of target compounds to the GC column when applying injection volumes of 0.2 microl, 1 microl, 2 microl, and 4 microl with splitless injection respectively 1 microl with split injection (split ratio, 1:40) were compared. It was demonstrated that splitless injections of 1 microl, 2 microl, and 4 microl could be employed in the developed method, while split injection and splitless injections of 0.2 microl should be avoided.

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