Peak compression in semi-preparative supercritical fluid chromatography

Abstract

Peak compression of a dihydropyridine drug, clevidipine, is obtained in both analytical and semi-preparative scale supercritical fluid chromatography, resulting in extremely high apparent efficiencies. The observed effect, when utilising a carbon dioxide/2-propanol mobile phase with a bare silica stationary phase, is achieved when the retention of the clevidipine peak is controlled to coalesce with a system peak, generated as a result of having water in the sample. Apparent efficiencies of 350,000 and 170,000 plates meter−1 were obtained when 0.25 and 0.5 mg, respectively, are directly injected to a 200×4.6 mm ID 5 μm Hypersil silica packed column. The effect was extended to a semi-preparative system where apparent efficiencies in the region of 2,000,000 plates meter−1 were observed when 0.3 mg of a clevidipine sample containing 80% water was injected to a 250×10 mm I.D. column containing 5-μm Hypersil silica particles.