Synthesis And Research On The Chromatographic Performance Of Calix[4]arene Derivatized Chitosan Bonded Silica Stationary Phases

HPLC is an important branch of chromatography and has been widely used inrecent years. And the chromatographic column is the centre of HPLC, therefore theresearches on new stationary phase has important significance. Chitosan is obtainedfrom chitin which is widespread in natural, and this natural polymer has a largenumber of amino, hydroxyl, which make it has a very wide range of applications;Calixarene is a compound with high thermal stability and chemical stability, thecavity size is easy to adjust, the conformation and substituents could be controlledartificially, and it is easy to be modified. In this paper, the unique properties ofchitosan and calixarene were combined and we prepared calix[4]arene derivatizedchitosan bonded silica stationary phase, characterized and studied its chromatographicbehavior and methodology. Three contents were studied in this article:1. Calix[4]arene derivatized chitosan bonded silica stationary phase wasprepared, and elemental analysis, infrared spectroscopy, thermal gravimetricanalysis were used to characterize this stationary phase and satisfactory results wasobtained. The bonding amount of chitosan and calix[4]arene were9.07μmol/g and41.1μmol/g; The temperature of thermal decomposition was280℃, whichindicated that the stationary phase has good thermal stability.2. Mono-substituted benzene, phenols, nucleosides and so on were used asprobes of solute to study the chromatographic behavior of calix[4]arenederivatized chitosan bonded silica stationary phase. We also compared thechromatography behavior of CCS4with commercial C18, the experiment resultsshowed that CCS4interact with solutes not only by hydrophobic but also by somehydrophilic when separating nucleosides, and hydrogen bonding, π-π, inclusioneffect et al. The effect of temperature on the retention time was also studied, whichshowed that the higher the temperature, the shorter the retention time.3. Calix[4]arene derivatized chitosan bonded silica stationary phase was alsoused to determine the actual sample and study methodology. The results ofdetermination of PCBs (2,3,3’,4,4’,5–Hexachlorobiphenyl and2,2’,3,3’,4,5,6,6’-Octachlorobiphenyl) in environmental water and the pyrimidine in plasma (cytosine and uracil) showed there had a good linearity (r2>0.99), low detectionlimit (2,3,3’,4,4’,5–Hexachlorobiphenyl10ng/mL,2,2’,3,3’,4,5,6,6’－Octachlorobiphenyl20ng/mL, cytosine2×10-2ng/mL, uracil1×10-2ng/mL), goodreproducibility (RSD<0.209%), and the recovery was higher (2,3,3’,4,4’,5－Hexachlorobiphenyl72.1%－85.4,2,2’,3,3’,4,5,6,6’－Octachlorobiphenyl60.5%－77.3%, cytosine80.7%-107.2%, uracil83.6%-108.1%).