MISER chiral supercritical fluid chromatography for high throughput analysis of enantiopurity.

MISER chromatographic analysis (Multiple Injections in a Single Experimental Run) using supercritical fluid chromatography (SFC) with pressurized carbon dioxide-based eluents is well suited to the high throughput analysis of enantiopurity. SFC is currently the preferred method for fast enantiopurity analysis, with analysis times of only a few seconds achievable in some cases. Injector programming using both the Agilent Infinity and Shimadzu Nexera UC instruments permitted MISER SFC experiments to be performed. Several case studies are presented, showcasing the power and versatility of the technique, with 'plate analysis times' (the time required for analysis of enantiopurity of 96 samples) of less than 33-34 min achievable in the best cases.

[1]  O. Trapp,et al.  Implementation of Hadamard encoding for rapid multisample analysis in liquid chromatography. , 2015, Journal of separation science.

[2]  Kendall N Houk,et al.  Rapid catalyst identification for the synthesis of the pyrimidinone core of HIV integrase inhibitors. , 2012, Angewandte Chemie.

[3]  R. Kennedy,et al.  Droplet Electrospray Ionization Mass Spectrometry for High Throughput Screening for Enzyme Inhibitors , 2014, Analytical chemistry.

[4]  Jong Seung Kim,et al.  Chromogenic/Fluorogenic Ensemble Chemosensing Systems. , 2015, Chemical reviews.

[5]  C. Welch,et al.  Evaluation of capsaicin in chili peppers and hot sauces by MISER HPLC-ESIMS , 2014 .

[6]  D. Armstrong,et al.  High efficiency, narrow particle size distribution, sub-2 μm based macrocyclic glycopeptide chiral stationary phases in HPLC and SFC. , 2015, Analytica chimica acta.

[7]  Kevin Bateman,et al.  Nanomole-scale high-throughput chemistry for the synthesis of complex molecules , 2015, Science.

[8]  F. Gasparrini,et al.  Ultra-fast high-efficiency enantioseparations by means of a teicoplanin-based chiral stationary phase made on sub-2 μm totally porous silica particles of narrow size distribution. , 2016, Journal of chromatography. A.

[9]  C. Welch,et al.  Separation of achiral analytes using supercritical fluid chromatography with chiral stationary phases , 2015 .

[10]  C. Welch,et al.  Pushing the speed limit in enantioselective supercritical fluid chromatography. , 2015, Journal of separation science.

[11]  Lei You,et al.  Recent Advances in Supramolecular Analytical Chemistry Using Optical Sensing. , 2015, Chemical reviews.

[12]  C. Welch,et al.  Adsorbent Screening Using Microplate Spectroscopy for Selective Removal of Colored Impurities from Active Pharmaceutical Intermediates , 2008 .

[13]  John F. Hartwig,et al.  A Simple, Multidimensional Approach to High-Throughput Discovery of Catalytic Reactions , 2011, Science.

[14]  Richard M Crooks,et al.  Paper-based SlipPAD for high-throughput chemical sensing. , 2013, Analytical chemistry.

[15]  Xiaoyi Gong,et al.  Supercritical fluid chromatography for GMP analysis in support of pharmaceutical development and manufacturing activities. , 2016, Journal of pharmaceutical and biomedical analysis.

[16]  C. West Enantioselective Separations with Supercritical Fluids - Review , 2013 .

[17]  Christopher J. Welch,et al.  Microplate evaluation of process adsorbents , 2002 .

[18]  Alexei Lapkin,et al.  Automatic discovery and optimization of chemical processes , 2015 .

[19]  R. Papp,et al.  Evaluating MISER chromatography for a rapid formulation screen. , 2013, Journal of pharmaceutical and biomedical analysis.

[20]  W. Schafer,et al.  Improved chiral SFC screening for analytical method development. , 2013, Chirality.

[21]  Frank Glorius,et al.  Contemporary screening approaches to reaction discovery and development. , 2014, Nature chemistry.

[22]  Jimmy O. DaSilva,et al.  Adsorbent Screening for Metal Impurity Removal in Pharmaceutical Process Research , 2005 .

[23]  Christopher J. Welch,et al.  MISER chromatography (multiple injections in a single experimental run): the chromatogram is the graph , 2010 .

[24]  C. Welch,et al.  Estimating optimal time for fast chromatographic separations. , 2014, Journal of separation science.

[25]  D. Armstrong,et al.  Gone in seconds: praxis, performance, and peculiarities of ultrafast chiral liquid chromatography with superficially porous particles. , 2015, Analytical chemistry.

[26]  Davy Guillarme,et al.  Coupling state-of-the-art supercritical fluid chromatography and mass spectrometry: from hyphenation interface optimization to high-sensitivity analysis of pharmaceutical compounds. , 2014, Journal of chromatography. A.

[27]  W. Schafer,et al.  Chromatographic resolution of closely related species: separation of warfarin and hydroxylated isomers. , 2013, Journal of chromatography. A.

[28]  F. Gasparrini,et al.  Expanding the potential of chiral chromatography for high-throughput screening of large compound libraries by means of sub-2μm Whelk-O 1 stationary phase in supercritical fluid conditions. , 2015, Journal of chromatography. A.

[29]  E. Regalado,et al.  Development of a Direct Photocatalytic C-H Fluorination for the Preparative Synthesis of Odanacatib. , 2015, Organic letters.

[30]  O. Trapp,et al.  Development of a straightforward and robust technique to implement hadamard encoded multiplexing to high-performance liquid chromatography. , 2014, Analytical chemistry.

[31]  Caroline West,et al.  The many faces of packed column supercritical fluid chromatography--a critical review. , 2015, Journal of chromatography. A.

[32]  C. Welch,et al.  Observations of Rhodium‐Containing Reaction Intermediates using HPLC with ICP‐MS and ESI‐MS Detection , 2006 .

[33]  Olivier Jacquet,et al.  Cover Picture: A Diagonal Approach to Chemical Recycling of Carbon Dioxide: Organocatalytic Transformation for the Reductive Functionalization of CO2 (Angew. Chem. Int. Ed. 1/2012) , 2012 .