Pushing the speed limit in enantioselective supercritical fluid chromatography

The ever-increasing need for enantiomerically pure chiral compounds has greatly expanded the number of enantioselective separation methods available for the precise and accurate measurements of the enantiomeric purity. The introduction of chiral stationary phases for liquid chromatography in the last decades has revolutionized the routine methods to determine enantiomeric purity of chiral drugs, agrochemicals, fragrances, and in general of organic and organometallic compounds. In recent years, additional efforts have been placed on faster, enantioselective analytical methods capable to fulfill the high throughput requirements of modern screening procedures. Efforts in this field, capitalizing on improved chromatographic particle technology and dedicated instrumentation, have led to highly efficient separations that are routinely completed on the seconds time scale. An overview of the recent achievements in the field of ultra-high-resolution chromatography on column packed with chiral stationary phases, both based on sub-2 μm fully porous and sub-3 μm superficially porous particles, will be given, with an emphasis on very recent studies on ultrafast chiral separations.

Section: Introductionmentioning

confidence: 99%

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

Ciogli

Ismail

Mazzoccanti

et al. 2018

“…The use of SFC for enantioselective separations has become a welcome extension in the application field of SFC. For both analytical and preparative scale analyses, enantioseparation in SFC offers some advantages over HPLC . In combination with effective chiral stationary phases (CSPs), it is a potent tool that can be employed for separations of enantiomers in pharmaceutical laboratories, as well as environmental and food‐control labs .…”

Section: Introductionmentioning

confidence: 99%

“…in SFC offers some advantages over HPLC [1][2][3]. In combination with effective chiral stationary phases (CSPs), it is a potent tool that can be employed for separations of enantiomers in pharmaceutical laboratories, as well as environmental and food-control labs [4].…”

Section: Introductionmentioning

confidence: 99%

Cellulose tris‐(3,5‐dimethylphenylcarbamate)‐based chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography: comparison with HPLC

Kalíková

Martínková

Schmid

et al. 2018

A cellulose tris-(3,5-dimethylphenylcarbamate)-based chiral stationary phase was studied as a tool for the enantioselective separation of 21 selected analytes with different pharmaceutical and physicochemical properties. The enantioseparations were performed using supercritical fluid chromatography. The effect of the mobile phase composition was studied. Four different additives (diethylamine, triethylamine, isopropylamine, and trifluoroacetic acid) and isopropylamine combined with trifluoroacetic acid were tested and their influence on enantioseparation was compared. The influence of two different mobile phase co-solvents (methanol and propan-2-ol) combined with all the additives was also evaluated. The best mobile phase compositions for the separation of the majority of enantiomers were CO /methanol/isopropylamine 80:20:0.1 v/v/v or CO /propan-2-ol/isopropylamine/trifluoroacetic acid 80:20:0.05:0.05 v/v/v/v. The best results were obtained from the group of basic β-blockers. A high-performance liquid chromatography separation system composed of the same stationary phase and mobile phase of similar properties prepared as a mixture of hexane/propan-2-ol/additive 80:20:0.1 v/v/v was considered for comparison. Supercritical fluid chromatography was found to yield better results, i.e. better enantioresolution for shorter analysis times than high-performance liquid chromatography. However, examples of enantiomers better resolved under the optimized conditions in high-performance liquid chromatography were also found.

“…Flow rate 3 mL/min or 2.3 mL/min so as to keep the same linear velocity on all columns. Adapted from with permission from Wiley.…”

Section: Use Of Chiral Sfc For Analytical Purposesmentioning

confidence: 99%

Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification

Lemasson

Bertin

West

2016

101

The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered.