Titania-coated fibrous silica (TiO2/KCC-1) core-shell microspheres based solid-phase extraction in clam (Corbicula fluminea) using hydrophilic interaction liquid chromatography and mass spectrometry.

Clam (Corbicula fluminea) contains significant amount of phospholipids, and the profile of phospholipids could be used as an index for nutrition evaluation. In this study, a titania-coated fibrous silica (TiO2/KCC-1) core-shell microsphere based solid-phase extraction (SPE) and hydrophilic interaction liquid chromatography mass spectrometry (HILIC-MS) method was developed to study the phospholipids in clam. The structure and morphology of TiO2/KCC-1 were characterized by transmission electron microscopy (TEM), scanning electron microscope (SEM), X-ray diffraction (XRD), and ultraviolet-visible diffuse reflectance spectroscopy (UV-vis DRS). The analytical results indicated that the phospholipid molecular species (PMS) could be extracted in a cleaner manner after TiO2/KCC-1 SPE, benefiting from the enhanced signals and decreased MS noise of phospholipids. Based on the principal component analysis (PCA) and partial least squares regression discriminant analysis (PLS-DA) models, the PMS with the most obvious beneficiaries of TiO2/KCC-1 SPE were identified, e.g. PC 16:0/20:5 (m/z 824.6), PC 16:0/22:6 (m/z 850.6), PE 18:1/18:2 (m/z 740.4), and PE 18:0/22:6 (m/z 790.5). Finally, the proposed method was validated to be sensitive and precise. This study provides an efficient tool to analyze the phospholipids in clam and the prospect to use this method for future applications in various samples.