Desorption mass spectrometry of olestra

Abstract

Field desorption (FD), fast atom bombardment (FAB) and plasma desorption (PD) mass spectrometry have been used for the characterization of olestra, a mixture of octa‐, hepta‐ and hexaesters of sucrose formed by reaction of sucrose with long‐chain fatty acids (C12–C18). Most previous applications of desorption ionization mass spectrometry have involved polar compounds; however, the relatively low‐polarity olestra is also amenable to these techniques with proper sample preparation. Field desorption provides molecular weight information, but the transience of the signals limits the usefulness for observing fragmentation and measuring ester distributions. In addition, FD may not be sensitive enough to allow characterization of fractions isolated from analytical high‐performance liquid chromatography (HPLC) columns. Fast atom bombardment produces longer‐lasting signals, which permit characterization of components over a wide mass range. However, signal‐to‐noise fluctuates substantially, depending on analyte solubility in the matrix, making the characterization of partial esters collected from HPLC uncertain and difficult. Plasma desorption mass spectrometry is the easiest and most sensitive technique for olestra characterization but provides the lowest mass resolution. Because it requires no more than a few µg of material, it is effective for the characterization of HPLC fractions. Furthermore, it is the only method, of the three investigated, that allows detection of intact dimeric species having molecular masses in the 3,000 to 5,000 dalton range.