Nanoparticle-based polyacrylonitrile monolithic column for highly efficient micro solid-phase extraction of carotenoids and vitamins in human serum.

In this work, a biocompatible monolithic column based micro-solid-phase extraction (µ-SPE) method was developed for biological fluid analysis. A novel nanoparticle-based polyacrylonitrile monolithic column (C30 NP-PMC) was fabricated by incorporating triacontyl (C30) modified silica nanoparticles (NPs) into the polyacrylonitrile monolithic matrix through thermally induced phase separation. With efficient mass transfer and sorption capacity, C30 NP-PMC exhibited outstanding performance for the extraction of carotenoids and fat-soluble vitamins (FSVs) from human serum samples, superior to commercial C18 cartridges as well as liquid-liquid extraction (LLE) method. Under optimal conditions, the proposed µ-SPE method coupled with high-performance liquid chromatography-diode array detection (HPLC-DAD) achieved satisfactory limits of detection (LODs) (1.5-75.0 ng/mL) and good recoveries (85.0-106.5 %) with relative standard deviations (RSDs) of less than 12.1% by consuming lower sorbent (35.0 mg) and organic solvent (0.8 mL). Successful application of the developed method demonstrated the great potential of such monolithic sorbents for efficient isolation and preconcentration of trace analytes from blood samples.