Eke, Zs.

Horváth, Simon

Ilisz, István

Németh, G.

Péter, A.

Horváth Simon

Eke Zs.

Péter A.

Ilisz István

Németh G.

University of Szeged

 25th International Symposium on Analytical and Environmental Problems 81 SWAP BETWEEN NORMAL PHASE AND POLAR ORGANIC MODE ON ADMPC CHIRAL STATIONARY PHASES  Horváth, S.1,2, Eke, Zs.3,4, Péter, A.5, Ilisz, I.5, Németh, G.1  1Egis Pharmaceuticals PLC, Drug Substance Development Division, H-1475 Budapest, Keresztúri út 30-38, Hungary 2Eötvös Loránd University, György Hevesy Doctoral School of Chemistry, H-1117 Budapest, Pázmány Péter sétány 1/A, Hungary 3Eötvös Loránd University, Joint Research and Training Laboratory on Separation Science, H-1117 Budapest, Pázmány Péter sétány 1/A, Hungary 4Wessling International Research and Educational Center, H-1045 Budapest, Anonymus u. 6, Hungary 5Institute of Pharmaceutical Analysis, University of Szeged,  H-6720 Szeged, Eötvös u. 6, Hungary e-mail: horvath.simon@egis.hu  Abstract Investigation of enantiomers is a common and important task in the pharmaceutical industry. In vast majority of the cases direct HPLC methods are used with polysaccharide-based chiral stationary phases [1-3]. The reason behind their versatility is the fact that many different chiral environments are accessible on them, due among others to their multimodal nature.  In continuation to our studies about the characterization [4] and the practical assessment of some history dependent chiral chromatographic systems in the polar organic (PO) mode, we extended our investigations to normal phase (NP). We found that an amylose tris(3,5-dimethylphenylcarbamate) (ADMPC) based column in the alkane-IPA systems exhibited hysteresis phenomenon. The effect can be observed both in heptane-IPA and hexane-IPA systems, and it is in close alignment with the known cost-increasing issue in chiral HPLC, namely that the reproduction of the retentions after swapping the modes is often problematic with polysaccharide-based columns. To avoid this undesirable consequence, column manufacturers advise to dedicate polysaccharide-based chiral columns to eluent modes. However, we discovered that by a quick rinse with a particular alcohol mixture the normal phase column test of the manufacturer can be reproduced after using the column in polar organic mode. We also found that heptane/IPA mixtures can be used indefinitely, without losing the purchased selectivity, if the IPA content does not exceed 70%.  References [1] J. Shen, Y. Okamoto, Chem. Rev. 116 (2016) 1094-1138. [2] B. Chankvetadze, J. Chromatogr. A 1269 (2012) 26-51. [3] E. Francotte, LCGC Europe 29 (suppl) (2016) 31-37. [4] S. Horváth, G. Németh, J. Chromatogr. A 1568 (2018) 149-159.   

Swap between normal phase and polar organic mode on ADMPC chiral stationary phases

http://acta.bibl.u-szeged.hu/64782/1/proceedings_of_isaep_2019_081.pdf

Swap between normal phase and polar organic mode on ADMPC chiral stationary phases

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