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A method for the preparation of poly(N‐vinylpyrrolidone‐co‐pentaerythritol triacrylate copolymerization)‐based monolithic capillary column was reported for the separation of polar small molecular weight compounds with nano‐liquid chromatography in hydrophilic interaction chromatography mode. The monolithic columns were prepared by in situ copolymerization of N‐vinylpyrrolidone and a cross‐linker pentaerythritol...