Superficially Porous Particle Based Hydroxypropyl‐β‐cyclodextrin Stationary Phase for High‐Efficiency Enantiomeric Separations

Abstract

A superficially porous particle (SPP)-based hydroxypropyl-β-cyclodextrin (HPBCD) chiral stationary phase (CSP) was produced and its chromatographic performance was compared to both 5 µm and 3 µm fully porous particle (FPP)-based CSPs. The relative surface coverage of the HPBCD chiral selector on each particle was approximately equal, which resulted in equivalent enantiomeric selectivity (α) values on each phase when constant mobile phase conditions were used. Under such conditions, the SPP column resulted in greatly reduced analysis times and three times greater efficiencies compared to the FPP columns. When higher flow rates were used, efficiency gains per analysis times were five times greater for the SPP column compared to the FPP-based columns. When the mobile phases were altered to give similar analysis times on each column, resolution values were doubled for the SPP column. Finally, the novel SPP based HPBCD column proved to be stable for 500 injections under high flow rate (4.5 mL/min) and high pressure (400 bar) conditions used for an ultrafast (~45 sec) enantiomeric separation.

Sampling frequency, response times and embedded signal filtration in fast, high efficiency liquid chromatography: A tutorial

“…Even today's state of the art high performance instruments can potentially limit the "true" performance of a chromatography column. In our experience as well as that of others [3,5,[10][11][12][13], even current generation instrumentation can contribute as much as 30-60% to peak variance for short, narrow bore columns. Remedial focus is often on injection ports and connections tubing as these are easily changed.…”

Enantioselective ultra high performance liquid and supercritical fluid chromatography: The race to the shortest chromatogram

“…Armstrong and co‐workers undoubtedly offered a wide comprehensive work in evaluation of SPPs for chiral separations. They bonded hydroxypropyl‐β‐cyclodextrin, cyclofructan‐6 based selectors, teicoplanin, its aglycone, and vancomycin on 2.7 μm SPPs . Focusing on the kinetic behavior, they showed the chiral SPPs outperform their FPPs counterparts in all working conditions ranging from normal phase to polar organic mode to HILIC.…”

Recent Advances in Chromatography for Pharmaceutical Analysis

“…Hydroxypropyl-β-cyclodextrin, cyclofructan-6 based selectors, teicoplanin, and vancomycin were also recently bonded on 2.7 μm SPPs. [210][211][212][213] It was found that chiral SPPs Chiral separations are still one of the workhorses for SFC since the analysis and production of enantiomerically pure compounds is still a major topic of interest when active pharmaceutical ingredients are concerned. There are a lot of improvements that were brought to chiral SFC analysis thanks to the use of modern systems and columns packed with small particles.…”