Instrumental considerations for the effective operation of short, highly efficient fused-core columns. Investigation of performance at high flow rates and elevated temperatures

摘要

Fused core or superficially porous columns offer the advantages of higher efficiency compared with totally porous columns of the same particle size, but similar operating pressures. However, their performance may be adversely affected by extra-column effects that become more significant as the column efficiency increases, and as the diameter of the column is reduced. In this study, we show that 10 cm × 0.46 cm fused-core columns can be used on modified conventional instruments (" microbore systems") without serious loss in performance, and this approach is at present likely to yield superior results compared with use of 0.21. cm columns (of identical efficiency) on current UHPLC instruments that have minimised extra-column volume. Furthermore, the true efficiency of commercial narrow-bore fused-core columns appears to be reduced compared with those of conventional bore, which may be due to packing difficulties for the former type. The fused-core columns in general gave excellent performance, showing no evidence of an upturn in the Knox plots at high flow velocities and elevated temperatures. Careful control of experimental conditions is necessary to ensure accurate data for these plots.