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Scanning electron, fluorescence, and atomic force microscopy techniques showed the formation of a relatively rough layer of polymer. In addition, \u2013CN and C\u00a0=\u00a0O stretching vibrations from infrared spectroscopy proved the successful immobilization of the azo\u2010initiator through covalent bonding and X\u2010ray\u00a0photoelectron\u00a0spectroscopy confirmed the elemental composition of the formed polymer layer. The prepared column was found to be appropriate for small and medium\u2010sized molecules separation. Compared to bare fused silica capillary column higher selectivity and resolution were obtained for the separation of alkaloids, sulfonamides, and peptides as a result of the electrostatic and pi\u2010pi stacking interactions between the small organic molecules and the coated column without compromising the electroosmotic flow mobility. Separation efficiency was also increased compared to the bare capillary for the separation of alkaloids (about 1.5 times). Moreover, intraday, inter\u2010day, intra\u2010batch, and inter\u2010batch relative standard deviation values of retention time and peak area of peptides were within 2% and 10%, respectively, indicating good repeatability of the column preparation procedure. The developed method for the covalent bonding of polymers through a functionalized azo\u2010initiator could represent a promising stable method for the preparation of an open tubular column.<\/jats:p>","DOI":"10.1002\/jssc.202200711","type":"journal-article","created":{"date-parts":[[2023,3,17]],"date-time":"2023-03-17T07:37:23Z","timestamp":1679038643000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Preparation of open tubular capillary column covalently coated with polystyrene sulfonate with 4,4\u2032\u2010Azobis(4\u2010cyanopentanoyl chloride) as polymerization initiator for electrochromatographic separation of alkaloids, sulfonamides, and peptides"],"prefix":"10.1002","volume":"46","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-3354-2397","authenticated-orcid":false,"given":"Vinay","family":"Naithani","sequence":"first","affiliation":[{"name":"School of Pharmacy Shanghai Jiao Tong University  Shanghai P. 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