Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1218, Issue 9, Pages 1266-1272Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.chroma.2010.12.120
Keywords
Pseudoephedrine; Ephedrine; Artifact; Gas chromatography; MTBSTFA; Doping
Funding
- Fundacao Universitaria Jose Bonifacio-FUJB
- CNPq
- FAPERJ
- CBF
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The compound 3,4-dimethyl-5-phenyl-1,3-oxazolidine can appear as an artifact during the gas chromatographic analysis of ephedrines. Its presence is a risk for doping control and forensic analyses. An evaluation about the consequences of its formation showed the possibility of a false positive for ephedrine, a false negative for pseudophedrine and increased uncertainty in the quantitative approach. Misinterpretations can be avoided with the observation of fragments m/z 56 and 71 in the ephedrine mass spectrum during GC-MS analysis and also by the formation of N-TFA-O-TBDMS derivatives prior to GC analysis. These N-TFA-O-TBDMS derivatives lead to an increase in the number and mass of diagnostic ions, meet the identification criteria, and provide an improvement in chromatographic resolution, allowing the separation of the ephedrines. (C) 2011 Elsevier B.V. All rights reserved.
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