This study describes the development and validation of a fast, accurate, and precise UPLC-Q-TOF-MS method for the analysis of steryl glycosides (SGs). The best combination of separation and sensitivity was obtained with a methanol/water gradient and formic acid as additive, using electrospray ionization (ESI). SGs were detected almost exclusively as sodiated adducts, allowing identification of the intact molecule, including the sugar moiety. The TOF-MS system offered high mass accuracy (1.3 ppm), providing a valuable tool for SG identification. The method was used to quantify single SG species in oat bran and whole wheat, and it was demonstrated that reliable quantification requires accounting for the matrix effect, which may reduce the SG signal by up to 50% in some samples. The level of matrix effect also depends on food matrices with various SG contents, indicating that it should be individually considered for each sample.
Keywords: mass spectrometry; quadrupole time-of-flight; steryl glycosides; ultraperformance liquid chromatography.