Derivatization in Mass Spectrometry—1. Silylation

Abstract

This is the first of a series of reviews on the application of derivatization in mass spectrometry. A description is given of advances in silylation as a powerful tool used for increasing the volatility, thermal and thermo-catalytic stability, and chromatographic mobility of polar and unstable organic compounds. In addition to chemical aspects of silylation, mass spectral properties of silyl derivatives useful for structure determination and quantitation of various organic and biologically-active compounds, mainly by GC/MS, are described. Practically all tested and widely used silylating agents are described. The role of comprehensive libraries containing reference mass spectra for various silyl derivatives and search systems in structure determination is emphasized. Applications of silylation for particular analyses are summarised.

The Metabolic Origins of Mannose in Glycoproteins

“…The aqueous layer was separated and dried. The resulting solid was derivatized in the same manner as that described under "Sugar Phosphate Analysis" (17). For quantitation of glucose and mannose, the total ion count peak area of the respective Z-and E-forms of the sugars, or specific mass ions, was used for calculation based on standard curves.…”

Targeted Metabolite Profiling: Sample Preparation Techniques for GC-MSBased Steroid Analysis

“…[66][67][68] Diazomethane in diethyl ether (0.5 mL) was used to esterify steroid glucuronides from biological extracts followed by silylation with N-methyl-N-trifluoroacetamide (MSTFA)/TMCS (100:1 v/v).…”

Screening of phenolic substances in the Nordic environments

“…After capping the vial, the sample was heated to 60 °C for 30 min. Silylation as a tool for derivatization in mass spectrometry has recently been reviewed by Halket & Zaikin (2003).…”