Consequences of the formation of 3,4-dimethyl-5-phenyl-1,3-oxazolidine on the analysis of ephedrines in urine by gas chromatography and a new method for confirmation as N-trifluoroacetyl-O-t-butyldimethylsilyl ether derivatives
| Autor: | F.R. Aquino Neto, Henrique Marcelo G. Pereira, Vinicius Figueiredo Sardela, Patrícia D. O. Sardela |
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| Rok vydání: | 2010 |
| Předmět: |
Ephedrine
Oxazolidine Chromatography Chromatography Gas Resolution (mass spectrometry) Silylation Chemistry Fluoroacetates Organic Chemistry General Medicine Silanes Biochemistry Analytical Chemistry Nasal decongestant chemistry.chemical_compound Mass spectrum Linear Models Trifluoroacetic Acid Gas chromatography Gas chromatography–mass spectrometry Derivatization Artifacts Oxazoles Ethers |
| Zdroj: | Journal of chromatography. A. 1218(9) |
| ISSN: | 1873-3778 |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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