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Synthesis of a polyrotaxane‐based macroporous polymer as stationary phase for capillary electrochromatography via host–guest complexation of N , N ′‐ethylenedianilinediacrylamide with statistically methylated β‐cyclodextrin
Author(s) -
Wahl Annika,
AlRimawi Fuad,
Schnell Ingo,
Kornysova Olga,
Maruska Audrius,
Pyell Ute
Publication year - 2008
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700632
Subject(s) - chemistry , cyclodextrin , aqueous solution , copolymer , monomer , nuclear magnetic resonance spectroscopy , capillary electrochromatography , acrylamide , polymer , two dimensional nuclear magnetic resonance spectroscopy , hydrophobic effect , polymer chemistry , organic chemistry , chromatography , stereochemistry , capillary electrophoresis
A synthetic route to acrylamide‐based monolithic stationary phases for CEC with rotaxane‐type immobilized derivatized β‐CD was explored. N , N ′‐Ethylenedianilinediacrylamide was synthesized as the water‐insoluble crosslinker forming water‐soluble inclusion complexes with statistically methylated β‐CD. Mixed‐mode stationary phases were synthesized by free radical copolymerization of the bisacrylamide‐CD host–guest complex with water‐soluble monomers and an additional water‐soluble crosslinker in aqueous solution. Complex formation in solution and inclusion of the pseudorotaxane into the polymeric network (formation of a polyrotaxane architecture) were studied by means of 1 H‐NMR chemical shift analysis, CD modified micellar EKC (CD‐MEKC), 2D‐NOESY spectroscopy, and solid state 13 C‐NMR spectroscopy. The presence of a mixed‐mode selectivity of the stationary phase based on hydrophobic and hydrophilic interaction was confirmed by CEC with neutral polar and nonpolar solutes.