Use of synthetic adsorbents in preparative normal-phase liquid chromatography

Abstract

Normal-phase liquid chromatographic separation using polymeric synthetic adsorbents was investigated. The retention behavior of dialkyl phthalates under a hexane–isopropanol eluent system revealed that both polystyrenic and polymethacrylic adsorbents can be used for normal-phase liquid chromatography, and that the polymethacrylic adsorbent has stronger retentivity than the polystyrenic adsorbent. Applicability of these synthetic adsorbents, especially the polymethacrylic adsorbents, was verified by the separation of polyunsaturated fatty acids, schizandrin in Schisandra chinensis fruit, tocopherols and tocotrienols in vegetable oils using a 10-μm adsorbent packed into an HPLC column. Furthermore, the separation was expanded to preparative scale by using polymethacrylic adsorbents with 17- and 31-μm fine grade particle sizes. The effect of loading volume on the retention or separation was also examined, and separation was maintained up to the loading of several grams per liter adsorbent. These results demonstrate that commercially available synthetic adsorbents possess considerable performance as normal-phase chromatographic media for more precise purification of bioactive compounds, including pharmaceuticals and nutraceuticals with scale-up possibilities.