| Abstract: | Macroscopic monoliths are highly desirable in many fields of application. Herein, well organized organic–inorganic cryogel composite with a three‐dimensional hierarchical meso‐ and macroporous structure are presented, which were produced by in situ copolymerization of mesoporous multifunctional silica (size: 1–20 μm; pore: 2–20 nm mostly) and monomers (hydroxyethyl methacrylate and diallyldimethylammonium chloride) in water below the freezing point. This copolymerization method effectively adjusted the macropores of the basic cryogel, and the nanosilica was more homogeneously dispersed in the basic cryogel. The specific surface area of the cryogel composite was increased 17 times versus than that of the basic cryogel. The abundant meso‐ and macroporous pores on the cryogel composite provided sufficient reactive sites favorable for the efficient mass transport of target compounds. When the cryogel composite, as solid phase extraction adsorbent, was coupled with high‐performance liquid chromatography, an analytical tool, the nucleosides were quantified with good selectivity, lower detection limits (0.9–1.3 ng/mL) and satisfactory recoveries of greater than 80% from spiked human serum. |
