Preparation of a novel carboxyl stationary phase by "thiol-ene" click chemistry for hydrophilic interaction chromatography.

A novel carboxyl-bonded silica stationary phase was prepared by "thiol-ene" click chemistry. The resultant Thiol-Click-COOH phase was evaluated under hydrophilic interaction liquid chromatography (HILIC) mobile phase conditions. A comparison of the chromatographic performance of Thiol-Click-COOH and pure silica columns was performed according to the retention behaviors of analytes and the charged state of the stationary phases. The results indicated that the newly developed Thiol-Click-COOH column has a higher surface charge and stronger hydrophilicity than the pure silica column. Furthermore, the chromatographic behaviors of five nucleosides on the Thiol-Click-COOH phase were investigated in detail. Finally, a good separation of 13 nucleosides and bases, and four water-soluble vitamins was achieved.

Online profiling of triacylglycerols in plant oils by two-dimensional liquid chromatography using a single column coupled with atmospheric pressure chemical ionization mass spectrometry.

The complexity of natural triacylglycerols (TAGs) in various edible oils is high because of the hundreds of TAG compositions, which makes the profiling of TAGs quite difficult. In this investigation, a rapid and high-throughput method for online profiling of TAGs in plant oils by two-dimensional (2D) liquid chromatography using a single column coupled with atmospheric pressure chemical ionization (APCI) mass spectrometry was reported. A novel mixed-mode 2D chromatographic column packed with silver-ion-modified octyl and sulfonic co-bonded silica was employed in this online 2D separation system. This novel 2D column combined the features of C8 column and silver-ion. In comparison with the traditional C18 column and silver-ion column, which are the two main columns used for the separation of complex TAGs in natural oil samples, this novel 2D column, could provide hydrophobic interactions as well as π-complexation interactions. It exhibited much higher selectivity for the separation of TAGs, and the separation was rapid. This online 2D separation system was successful in the separation of a large number of TAG solutes, and the TAG structures were evaluated by analyzing their APCI mass spectra information. This system was applied for the profiling of TAGs in peanut oils, corn oils, and soybean oils. 30 TAGs in peanut oils, 18 TAGs in corn oils, and 21 TAGs in soybean oils were determined and quantified. The highest relative content of TAGs was LLL, which was found in corn oil with the relative content up to 45.43 (%, w/w), and the lowest relative content of TAGs was LLS and OSS, which was found in soybean oil and corn oil respectively, with the relative content only 0.01 (%, w/w). In addition, the TAG data were analyzed by principal component analysis (PCA). Results of PCA enabled a clear identification of different plant oils. This method provided an efficient and convenient chromatographic technology for the fast characterization and quantification of complex TAGs in plant oils at high selectivity. It has great potential as a routine analytical method for analysis of edible oil quality and authenticity control.