PMID- 34074384 OWN - NLM STAT- PubMed-not-MEDLINE DCOM- 20210602 LR - 20210602 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 232 DP - 2021 Sep 1 TI - High efficiency functionalized hydrophilic cyclofructans as stationary phases in sub/supercritical fluid chromatography. PG - 122308 LID - S0039-9140(21)00229-0 [pii] LID - 10.1016/j.talanta.2021.122308 [doi] AB - Packed column SFC has become very popular for preparative and analytical separations due to the low cost of CO(2), its accessible critical temperature, and pressure, with the additional benefit of a low environmental burden. Currently, there is a shortage of new polar stationary phase chemistries for SFC. In this work, two new functionalized cyclofructan columns are introduced and evaluated for their performance in achiral SFC separations for the first time. Cyclofructan (CF6), a macrocyclic oligosaccharide, was covalently linked with benzoic acid (BCF6) and propyl sulfonic acid (SCF6) groups by ether bonds. Superficially porous particles (2.7 mum) bonded with modified CF6 showed markedly different selectivity than native CF6. In SFC, peak shapes of amines and basic compounds are often compromised. We show that small quantities (~5.7% v/v) of water added to the methanol modifier in CO(2) improves peak symmetries of primary, secondary, and tertiary amines. Efficiencies as high as 200,000 plates/m (reduced plate height ~ 1.8) were observed for benzamide and amitriptyline on the BCF6 column. The relative standard deviations (RSDs) of retention times on BCF6 were about 1.4%, and on SCF6 were less than 1%. Amines on the SCF6 column showed plate counts as high as 170,000 plates/m. Tetramethylammonium acetate is examined as an alternative to water in MeOH. A run time of 36 min with methanol, trifluoroacetic acid, triethylamine mobile phase was reduced to <5 min with complete baseline resolution for a set of amines. The new stationary phases allow greener approaches towards solving separation problems. CI - Copyright (c) 2021 Elsevier B.V. All rights reserved. FAU - Firooz, Sepideh Khaki AU - Firooz SK AD - Department of Chemistry & Biochemistry, University of Texas at Arlington, TX, 76019, USA. FAU - Wahab, M Farooq AU - Wahab MF AD - Department of Chemistry & Biochemistry, University of Texas at Arlington, TX, 76019, USA. FAU - Yu, Jeongjae AU - Yu J AD - Department of Chemistry & Biochemistry, University of Texas at Arlington, TX, 76019, USA. FAU - Armstrong, Daniel W AU - Armstrong DW AD - Department of Chemistry & Biochemistry, University of Texas at Arlington, TX, 76019, USA. Electronic address: sec4dwa@uta.edu. LA - eng PT - Journal Article DEP - 20210318 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R SB - IM OTO - NOTNLM OT - Amines OT - Aqueous additives OT - Column efficiency OT - Derivatized cyclofructan OT - Drugs OT - Supercritical fluid chromatography OT - Superficially porous particles EDAT- 2021/06/03 06:00 MHDA- 2021/06/03 06:01 CRDT- 2021/06/02 05:41 PHST- 2021/01/25 00:00 [received] PHST- 2021/03/08 00:00 [revised] PHST- 2021/03/11 00:00 [accepted] PHST- 2021/06/02 05:41 [entrez] PHST- 2021/06/03 06:00 [pubmed] PHST- 2021/06/03 06:01 [medline] AID - S0039-9140(21)00229-0 [pii] AID - 10.1016/j.talanta.2021.122308 [doi] PST - ppublish SO - Talanta. 2021 Sep 1;232:122308. doi: 10.1016/j.talanta.2021.122308. Epub 2021 Mar 18.