N-trifluoracetyl-o-trimethylsilyl-phenolalkylamine : Darstellung und massenspezifischer gaschromatographischer nachweis
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Modern Sample Preparation for Chromatography
2021, Modern Sample Preparation for ChromatographyIdentification of sympathomimetic alkylamine agents in urine using liquid chromatography-mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography-mass spectrometry
2013, Journal of Chromatography ACitation Excerpt :Therefore, to minimize this adverse effect, MBTFA is used in small amounts in combination with large amounts of another derivatizing reagent. The concomitant use of MBTFA and MSTFA has been described for hydroxylamines [36–38], and the concomitant use of MBTFA and MTBSTFA was recently described by Sardela et al. [39] as a confirmatory procedure for ephedrines. Double derivatization using MSTFA and MBTFA was also investigated for alkylamines.
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
2011, Journal of Chromatography ACitation Excerpt :Therefore GC–MS analyses adopting derivatization strategies are currently used to increase the mass of the fragments, to add other diagnostic ions for structural characterization, and also to improve the chromatographic peak shapes. However, the strategy of double derivatization, to form N-TFA-O-TMS derivatives, reported by Donike [23] (Fig. 3b) and other derivatives for ephedrines [24,25] (Fig. 3c and d), do not show mass spectra with more than three ions as would be required for current identification criteria [26–28]. The aim of the present work is to characterize the unknown peak, potentially co-eluting with ephedrine, observed in our analyses and other doping control laboratories, and to determine its origin and the variables that may enhance its presence.
Analysis of sibutramine metabolites as N-trifluoroacetamide and O-trimethylsilyl derivatives by gas chromatography-mass spectrometry in urine
2009, Journal of Chromatography B: Analytical Technologies in the Biomedical and Life SciencesChapter 21 Doping substances in human and animal sport
2008, Handbook of Analytical SeparationsCitation Excerpt :The preparation of suitable derivatives, which give unique retention times, often provide additional information to help the identification of the compound present because the fragmentation pattern can be strongly altered [27]. The derivatisation technique commonly used is based on double derivatisation [23,59], where sequential addition of MSTFA and N-methyl-bis-trifluoroacetamide (MBTFA) gives the TMS derivatives of hydroxyl, acidic and phenolic groups and the TFA derivatives of primary and secondary amines [11,54,60]. These derivatives are very stable in solution and show excellent gas chromatographic properties.
Chapter 18 Chemical reactions used in derivatization
2002, Journal of Chromatography LibraryCitation Excerpt :Silylation with BSTFA of dopamine will generate a silylated derivative. Further reaction with MBTFA replaces the silyl group at the amino function but leaves unmodified the silyl groups at the hydroxyls [157], [158]. One other procedure successfully applied to obtain acyl derivatives is the use of acyl imidazoles as reagents.