Novel reactive matrices for analysis of alcohols by matrix-assisted laser desorption/ioization mass spectrometry
T15N2
M.S. Slyundina, R.S. Borisov, V.G. Zaikin
The possibility of using a number of aromatic and heteroaromatic carboxylic acids and their halogen anhydrides as reactive matrix compounds for the analysis of alcohols of different structures by matrix-assisted laser desorption/ionization (MALDI) mass spectrometry has been studied. It is shown that acylation of alcohols with nicotinic and quinoline-6-carboxylic acid chlorides makes it possible to obtain derivatives having a high desorption/ionization efficiency under MALDI conditions, and the free acids formed as a result of the hydrolysis of anhydrides act as matrix compounds. The proposed approach is tested on a number of aliphatic, alicyclic and aromatic alcohols.
Silylation with the generation of a fixed charge for the analysis of alcohols by MALDI and SALDI mass spectrometry
T15N1
D.I. Zhilyaev, L.G. Voskresensky, N.Yu. Polovkov, R.S. Borisov
A new method of derivatization of alcohols for their analysis by matrix-assisted laser desorption/ionization (MALDI) and surface-assisted laser desorption/ionization (SALDI) is proposed. The approach is based on the silylation of the analytes by bromomethylchlorodimethylsilane in the presence of tertiary amines to yield the fixed-charge containing derivatives. The proposed method was tested using aliphatic, terpenoid and steroid alcohols. MALDI and SALDI mass spectra of all derivatives contained intense ion peaks corresponding to their cationic parts.
A new post-chromatographic derivatization approach to identification of alcohols and phenols in complex mixtures by a combination of planar chromatography and matrix-assisted laser desorption/ionization mass spectrometry
T14N4
C.A. Esparza, N.Yu. Polovkov, R.S. Borisov, A.V. Varlamov, V.G. Zaikin
Simple and suitable approach for post-chromatographic derivatization in the analysis of mixtures of alcohols and phenols by combination of thin-layer chromatography and MALDI mass spectrometry was suggested for the first time. Chemical modification of analytes was accomplished by the treatment of eluted zones on thin-layer chromatograms by 3-bromopropionyl chloride in the presence of excess of a base (pyridine or triethylamine). The resulting derivatives contained a residue with fixed charge (ammonium fragment) that provided an efficient desorption of derivatized analytes from the sorbent layer during MALDI. It was shown that the suggested approach allows the recording of mass spectra with high signal/noise ratio and the detection of alcohols and phenols of different structures. Reproducibility of such MALDI mass spectra is rather high which predetermines a possibility to build the chromatogram curves using total or selected ion current and, hence, their visualization and treatment on quantitative level.
Simple and easy approach to derivatization of alcohols for the investigation by ‘soft’ ionization mass spectrometry methods
T11N2
R.S. Borisov, N.Yu. Polovkov, D.I. Zhilyaev, V.G. Zaikin
A.V. Topchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences
