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Chiral separation and quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in whole blood by GC-EI-MS.
J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Oct 02; 842(2):136-41.JC

Abstract

The enantioselective composition of the amphetamines is of interest, as the enantiomers show differences in their pharmacological effects and several methods for chiral separation of amphetamines have been described. Only a few methods have used whole blood as matrix and none of these separates both classic amphetamines (amphetamine and methamphetamine) and designer amphetamines (MDA, MDMA and MDEA). The aim of this study was, therefore, to develop a method for enantioselective analysis of AM, MA, MDA, MDMA, and MDEA in whole blood. The amphetamines were extracted from 0.5 g of whole blood by liquid-liquid extraction. After derivatization with R-MTPCl, the resulting diastereomers were separated by GC on a HP-5MS column and detected by SIM-MS. R-MTPCl was used as derivatization reagent because of the stability of this reagent and good separation of these analytes. Through the method, development time and temperature of the derivatization were optimized, and by admixture of 0.02% triethylamine it became possible to detect the amphetamines in adequately low concentrations as more analytes were derivatized. The method was validated and it was linear from 0.004 to 3 microg/g per enantiomer. The accuracy was within 91-115%, while the repeatability and reproducibility were < or =15% R.S.D. A method suitable for enantioselective separation and analysis of the amphetamines has been achieved, and the method was applied to analysis of whole blood samples originating from traffic and criminal cases and post mortem cases.

Authors+Show Affiliations

Department of Pharmaceutics and Analytical Chemistry, The Danish University of Pharmaceutical Sciences, Denmark.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

16797258

Citation

Rasmussen, Louise Bang, et al. "Chiral Separation and Quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in Whole Blood By GC-EI-MS." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 842, no. 2, 2006, pp. 136-41.
Rasmussen LB, Olsen KH, Johansen SS. Chiral separation and quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in whole blood by GC-EI-MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2006;842(2):136-41.
Rasmussen, L. B., Olsen, K. H., & Johansen, S. S. (2006). Chiral separation and quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in whole blood by GC-EI-MS. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 842(2), 136-41.
Rasmussen LB, Olsen KH, Johansen SS. Chiral Separation and Quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in Whole Blood By GC-EI-MS. J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Oct 2;842(2):136-41. PubMed PMID: 16797258.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Chiral separation and quantification of R/S-amphetamine, R/S-methamphetamine, R/S-MDA, R/S-MDMA, and R/S-MDEA in whole blood by GC-EI-MS. AU - Rasmussen,Louise Bang, AU - Olsen,Kristine Høje, AU - Johansen,Sys Stybe, Y1 - 2006/06/21/ PY - 2006/01/31/received PY - 2006/05/03/revised PY - 2006/05/09/accepted PY - 2006/6/27/pubmed PY - 2006/12/23/medline PY - 2006/6/27/entrez SP - 136 EP - 41 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J. Chromatogr. B Analyt. Technol. Biomed. Life Sci. VL - 842 IS - 2 N2 - The enantioselective composition of the amphetamines is of interest, as the enantiomers show differences in their pharmacological effects and several methods for chiral separation of amphetamines have been described. Only a few methods have used whole blood as matrix and none of these separates both classic amphetamines (amphetamine and methamphetamine) and designer amphetamines (MDA, MDMA and MDEA). The aim of this study was, therefore, to develop a method for enantioselective analysis of AM, MA, MDA, MDMA, and MDEA in whole blood. The amphetamines were extracted from 0.5 g of whole blood by liquid-liquid extraction. After derivatization with R-MTPCl, the resulting diastereomers were separated by GC on a HP-5MS column and detected by SIM-MS. R-MTPCl was used as derivatization reagent because of the stability of this reagent and good separation of these analytes. Through the method, development time and temperature of the derivatization were optimized, and by admixture of 0.02% triethylamine it became possible to detect the amphetamines in adequately low concentrations as more analytes were derivatized. The method was validated and it was linear from 0.004 to 3 microg/g per enantiomer. The accuracy was within 91-115%, while the repeatability and reproducibility were < or =15% R.S.D. A method suitable for enantioselective separation and analysis of the amphetamines has been achieved, and the method was applied to analysis of whole blood samples originating from traffic and criminal cases and post mortem cases. SN - 1570-0232 UR - https://www.unboundmedicine.com/medline/citation/16797258/Chiral_separation_and_quantification_of_R/S_amphetamine_R/S_methamphetamine_R/S_MDA_R/S_MDMA_and_R/S_MDEA_in_whole_blood_by_GC_EI_MS_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(06)00409-0 DB - PRIME DP - Unbound Medicine ER -