title: Single "click" synthesis of a mixed-mode silica sorbent and application in matrix solid-phase dispersion extraction of β-agonists from porcine liver.
abstract: A single "click" strategy is proposed for the preparation of a reversed-phase/weak cation-exchange mixed-mode silica-based sorbent (silica-WCX). Upon this strategy, both 1-dodecyne and 5-hexynoic acid were simultaneously immobilized onto azide-silica in varied ratio via Cu (I)-catalyzed azide-alkyne cycloaddition click reaction. The chemical compositions of silica-WCXs were characterized by elemental analysis, acid-base titration and Fourier transform-infrared spectroscopy. The results indicated that the actual mole ratio of n-dodecyl to carboxylic group on the sorbent is almost the same as the reactant ratio of 1-dodecyne to 5-hexynoic acid, and the repeatability of synthesis method is good. After that, two β-agonists, clenbuterol and ractopamine, were selected as model drug residues to evaluate the applicability of silica-WCX in matrix solid-phase dispersion extraction for the determination of basic drug residues in porcine liver by HPLC/UV. In comparison with some commercial sorbents, silica-WCX exhibited higher recoveries and better purification capability. Under the optimized conditions, linearity ranges were between 0.04 and 8.0μg/g for both analytes with coefficients of determination (R(2)) higher than 0.9997. The average recoveries at three spiked levels ranged from 92.5% to 105.0% with RSDs less than 6.6%.
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, Hubei, China.
authors.forename: Yuling
authors.initials: Y
authors.lastname: Zhu
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, Hubei, China.
authors.forename: Siwen
authors.initials: S
authors.lastname: Yang
authors.affiliation: Electric Power Research Institute of Guangdong Power Grid Corporation, Guangzhou, Guangdong, China.
authors.forename: Gang
authors.initials: G
authors.lastname: Chen
authors.affiliation: Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, Hubei, China. Electronic address: gc-ms@263.net.
authors.forename: Jun
authors.initials: J
authors.lastname: Xing
mesh_terms: D000318:Adrenergic beta-Agonists / Q000032:analysis*; D000818:Animals; D002976:Clenbuterol / Q000032:analysis*; D008099:Liver / Q000737:chemistry*; D010627:Phenethylamines / Q000032:analysis*; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000737:chemistry; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D017550:Spectroscopy, Fourier Transform Infrared / Q000295:instrumentation / Q000379:methods*; D013552:Swine
chemical_list: D000318:Adrenergic beta-Agonists; D010627:Phenethylamines; C060897:ractopamine; D012822:Silicon Dioxide; D002976:Clenbuterol
keywords: Click reaction; Matrix solid-phase dispersion; Mixed-mode; Reversed-phase/weak cation-exchange; β-Agonists