Preparation and application of sulfated lily polysaccharide bridged polyhedral oligomeric silsesquioxane hybrid organosilicas as stationary phase

Periodic mesoporous organosilicas (PMO) hydrophilic microspheres were synthesized by co-condensation of sulfated polysaccharide from Lilum lancifolium Thunb. bridged silane (SLLTPBS) and polyhedral oligomeric silsesquioxane (POSS) as stationary phase (PMO(SLLTP-POSS)) for per aqueous liquid chromatography (PALC), which would overcome the disadvantages of using a large amount of acetonitrile on the hydrophilic interaction liquid chromatography (HILIC) columns. Average particle size of PMO (SLLTP-POSS) microspheres was 4.9 μm, which was suitable for stationary phase. The retention mechanism of the stationary phase in PALC was mainly hydrophobic interactions and also included some ion-exchange interactions and electrostatic interactions. The acid-base resistance was greatly improved compared to the C18 column. The PMO(SLLTP-POSS) column under PALC mode had increased the resolution when separating some hydrophilic compounds such as eight organic acids and eleven sweeteners compared with the C18 column and HILIC column. The new column was more efficient than the HILIC columns. Additionally, a PALC-triple quadrupole mass spectrometry approach for the simultaneous identification of the eleven sweeteners was developed. The averagere coveries of the eleven compounds were 70.20%-91.33% with the relative standard deviation (RSD) range of 1.74% to 4.27%. The results showed good precision and accuracy of the method.