Monolithic silica columns with chemically bonded beta-cyclodextrin as a stationary phase for enantiomer separations of chiral pharmaceuticals.
An enantioselective silica rod type chiral stationary phase (CSP) is presented; a novel combination of the well known enantiomer separation properties of beta-cyclodextrin and the unique properties concerning the flow behavior of silica monoliths. Two different synthesis routes are described, and it was found that the in situ modification of a plain silica rod column turned out to be the best. The chromatographic behaviour of the beta-cyclodextrin silica rod was studied and compared with a very similar commercially available beta-cyclodextrin bonded particulate material (ChiraDex). Even if the amount of beta-cyclodextrin bound to the silica rod was only about half of the amount of beta-cyclodextrin bound to ChiraDex) particles, good resolutions were achieved for a set of chiral test components like Chromakalin, Prominal, Oxazepam, Methadone and some other drugs. By taking advantage of the unique features of the silica rods relating to their flat H/u (Van Deemter) curves, fast enantiomer separations could be demonstrated.
D002845:Chromatography / Q000295:instrumentation / Q000379:methods*; D003505:Cyclodextrins / Q000737:chemistry*; D006571:Heterocyclic Compounds / Q000737:chemistry / Q000302:isolation & purification; D008618:Mephobarbital / Q000737:chemistry / Q000302:isolation & purification; D008691:Methadone / Q000737:chemistry / Q000302:isolation & purification; D008855:Microscopy, Electron, Scanning; D009644:Norgestrel / Q000737:chemistry / Q000302:isolation & purification; D009930:Organic Chemicals / Q000737:chemistry / Q000302:isolation & purification; D010076:Oxazepam / Q000737:chemistry / Q000302:isolation & purification; D004364:Pharmaceutical Preparations / Q000737:chemistry / Q000302:isolation & purification*; D012822:Silicon Dioxide / Q000737:chemistry*; D013237:Stereoisomerism; D013696:Temperature; D013997:Time Factors
D003505:Cyclodextrins; D006571:Heterocyclic Compounds; D009930:Organic Chemicals; D004364:Pharmaceutical Preparations; D009644:Norgestrel; D008618:Mephobarbital; D010076:Oxazepam; D012822:Silicon Dioxide; D008691:Methadone