ABSTRACT
A method based on the analysis of trimethylsilyl (TMS) derivatives by capillary gas chromatography electrospray ionization mass spectrometry (GC-ESI/MS) was proposed. To improve separation, analytes were derivatized to their TMS derivative. During ESI analysis, TMS derivatives may hydrolyze back to their polar native form and are thus suitable for ESI analysis. Several types of analytes were studied to investigate the potential of the approach. Not all TMS derivatives hydrolyzed back to their native form as anticipated. Incomplete hydrolysis was observed for TMS-organic acids and TMS-nonchlorinated phenols. For TMS-chlorophenols, the observation of only the [M - H]- ion suggested that these phenols were hydrolyzed back to their native form. For TMS-beta agonists, the hydrolysis rate was low; therefore, the hydrolysis product was not detected. Both TMS-chlorophenols and TMS-beta agonists provide a sensitivity in the range of low parts per billion (0.25-5 ng/ml and 0.5-10 ng/ml respectively). Copyright © 2016 John Wiley & Sons, Ltd.
ABSTRACT
The trimethylsilyl (TMS) derivative is one of the most widely utilized derivatives for analyzing polar compounds by gas chromatography. An ion two mass units higher than the protonated molecular ion was observed in analyzing TMS-monocarboxylic acids by using gas chromatography electrospray ionization mass spectrometry (GC-ESI/MS). The structure of the M + 2 compound was investigated using tandem mass spectrometry and high-resolution mass spectrometry. The results suggest that one methyl group bound to the silicon atom was replaced by a hydroxyl group during the ESI process. One possible mechanism for the formation of the M + 2 compound is proposed. This observation suggests the possibility of synthesizing an organic compound by using ESI.
