Preparation And Chromatographic Characteristics Of Silia Based And β-CD Bonded Hplc Chiral Stitionary Phases

Enantioseparation of chiral compounds has been attracting burgeoning interests in the current century, which is partly attributed to their significantly differences in biological, pharmacological and toxicological effects. To date, high-performance liquid chromatography (HPLC) is perceived as the most common method employed for chiral separation of drug and pesticide enantiomers and a variety of chiral selectors are available. Among them, the functionalized β-cyclodextrin (β-CD) has attracted much attention on account of its effective stereoisomers separation ability via forming inclusion complexes with the analytes. Previously, research efforts were directed mainly on chemically anchoring cyclodextrin onto solid matrice via ether, amino, triazine spacer, the solvolytically more stable urea linkage and carbamic acid moieties. These approaches are not so satisfactory because they involve the use of some expensive raw materials and some hypertoxic, explosive or metal-containing catalysts. Furthermore, the preparation processes mostly involve the protection and deprotection of hydroxyl groups on the cyclodextrins, which make the synthesis routes tedious and complex. These factors, in part, may have contributed to the high cost and poor availability of the CD-CSPs.In this study, we report two facile approaches to synthetize silica based and P-CD bonded chiral stationary phase, which effectively overcome the above shortcomings. These totally porous silica microspheres were prepared via PICA method. The colloidal silica needed in this process was made from silica powder (99.9%) and SiCl4, which could ensure the high purity of HPLC column packing. Then, three kinds of β-CD bonded CSPs(CSP-Ⅰ/Ⅱ/Ⅲ) have been designed and synthesized with the5μm SiO2microspheres. At last, the chromatographic performance of these CSPs was achieved in HPLC under reversed-phase conditions with7kinds of chiral compounds, which involved two chiral drugs, four chiral pesticides and one chiral amino acid. On CSP-Ⅰ,2kinds of chiral compounds obtained baseline separation; On CSP-Ⅱ,4kinds of chiral compounds obtained baseline separation; On CSP-Ⅲ,4kinds of chiral compounds obtained baseline separation. All the retention time was less than10minutes, which means the CSPs prepared showed high anantioselectivity and wide separation range in the chiral separation process.