Preparation, Characterization And Application Of Silica-Bonded Tetraoxocalix "2" Arene "2" Triazine Stationary Phase For High Performance Liquid Chromatography

As the third-generation supermolecules after crown ethers and cyclodextrins, calixarenes are quite good molecule platforms, the structures of which are easily modified. Heterocalix[n]heteroarenes are synthesized from calixarene derivations, that is, the bridged carbon atoms of calixarenes are substituted by heteroatoms such as nitrogen,oxygen,sulfur,phosphorus et.al and phenol skeleton groups are substituted by aromatic heterocyclics such as furan,thiophene,indole,pyridine et.al. The introduction of bridged heteroatoms and aromatic heterocyclics bring great changes to structures and recognition performans of such macrocycles,compared to traditional calixarenes.This paper studied the preparation,characteration and chromatographic behaviors of silica-bonded tetraoxocalix[2]arene[2]triazine stationary phase and applied it to the determination of benzopyrene in environment samples and melamine in food,obtaining good results. This paper specifically included the following three parts:1 Silica-bonded tetraoxocalix[2]arene[2]triazine stationary phase was synthesized and characterized by IR, EA and TG. Analysis results showed that banding quantity was 0.367 mmol/g and thermal decomposition temperature was over 280℃, demonstrating that it had good thermal stability.2 The chromatographic behaviors of silica-bonded tetraoxocalix[2]arene[2]triazine stationary phase were investigated by using polycyclic aromatic hydrocarbons, positional isomers of hydroquinone,phenylenediamine and aminophenol, and several monosubstituted benzenes.When compared to commercial C18, the results showed that the new bonded stationary phase interact with solutes by hydrophobic as well as hydrogen bonding, p-p and inclusion effect et al.In addition,the melamine in milk samples obtained good separation and determination, which provided a new separation media and a new analysis method for the determination of melamine.3 The silica-bonded tetraoxocalix[2]arene[2]triazine stationary phase (TOA2T2) was applied to determinations of benzo(a)pyrene in air, soil and water by HPLC/FLD. The results are satisfactory with a good linear relationship in the range of 0.8-20 ng/mL(R2=0.999), good reproducibility (peak area RSD=2.55 %), detection limt 0.2ng/mL, recoveries 96%-101%.