title: Preparation of an internal surface reversed-phase restricted-access material for the analysis of hydrophobic molecules in biological matrices.
abstract: Restricted-access materials (RAMs) have been broadly used for sample pretreatment in the chromatographic analysis of biological samples. In the present work, a novel internal surface reversed-phase (ISRP) RAM was prepared via surface-initiated atom transfer radical polymerization (SI-ATRP). Octadecyl and 4-(chloromethyl)phenyl were immobilized on silica using a one-pot synthesis approach to form a reversed-phase layer to retain small hydrophobic molecules, allowing the modified silica to serve as a macro-initiator. Then, poly(glycidyl methacrylate) (pGMA) was grafted onto the surface via SI-ATRP, and the epoxy groups were further hydrolyzed to form an external hydrophilic layer. The properties of this ISRP-RAM for the retention of small molecules and the exclusion of proteins were evaluated using solid-phase extraction (SPE). The removal efficiencies of bovine serum albumin (BSA) and lysozyme were 94.9% and 93.5%, respectively. The recoveries of five drugs, puerarin, p-hydroxybenzaldehyde, loratadine, nifedipine and diazepam, were 93.2-116%. Furthermore, the ISRP-RAM was employed for the SPE of five phthalate esters (PAEs) from bovine milk prior to high-performance liquid chromatography (HPLC) analysis. The results indicate that the prepared ISRP-RAM is qualified for practical bioanalysis.
authors.affiliation: Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, 229 Tai Bai North Road, Xi'an 710069, Shaanxi, China. Electronic address: czwang@nwu.edu.cn.
authors.forename: Chaozhan
authors.initials: C
authors.lastname: Wang
authors.affiliation: Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, 229 Tai Bai North Road, Xi'an 710069, Shaanxi, China.
authors.forename: Ming
authors.initials: M
authors.lastname: Li
authors.affiliation: Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, 229 Tai Bai North Road, Xi'an 710069, Shaanxi, China.
authors.forename: Huanhuan
authors.initials: H
authors.lastname: Xu
authors.affiliation: Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, 229 Tai Bai North Road, Xi'an 710069, Shaanxi, China.
authors.forename: Yinmao
authors.initials: Y
authors.lastname: Wei
mesh_terms: D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057927:Hydrophobic and Hydrophilic Interactions; D008892:Milk / Q000737:chemistry; D058105:Polymerization; D012822:Silicon Dioxide / Q000737:chemistry; D052616:Solid Phase Extraction / Q000379:methods*; D017550:Spectroscopy, Fourier Transform Infrared; D013499:Surface Properties
chemical_list: D012822:Silicon Dioxide
keywords: Bioanalysis; Internal surface reversed phase; Phthalate esters; Restricted-access material; Solid-phase extraction