Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Marcel·lí Domingo s/n, Campus Sescelades, 43007 Tarragona, Spain.
J Chromatogr A. 2011 Jul 22;1218(29):4612-8. doi: 10.1016/j.chroma.2011.05.049. Epub 2011 May 23.
In this paper we describe the synthesis of a molecularly imprinted polymer (MIP) by precipitation polymerisation, with barbital as the template molecule, and the application of the barbital MIP as a molecularly selective sorbent in the solid-phase extraction (SPE) of barbiturates from human urine samples. The MIP was synthesised by precipitation polymerisation using 2,6-bis-acrylamidopyridine as the functional monomer and DVB-80 as the cross-linking agent. The spherical MIP particles produced were 4.2 ± 0.4 μm in diameter; a non-imprinted control polymer (NIP) in bead form was 4.8 ± 0.4 μm (mean±standard deviation) in diameter. The particles were packed into a solid-phase extraction cartridge and employed as a novel sorbent in a molecularly imprinted solid-phase extraction (MISPE) protocol. The MIP showed high selectivity for the template molecule, barbital, a feature which can be ascribed to the high-fidelity binding sites present in the MIP which arose from the use of 2,6-bis-acrylamidopyridine as the functional monomer. However, the MIP also displayed useful cross-selectivity for other barbiturates besides barbital. For real samples, the MIP was applied for the extraction of four barbiturates from human urine. However, due to the high urea concentration in this sample which interfere the proper interaction of barbiturates onto the MIP, a tandem system using a commercially available sorbent was developed.
本文描述了一种通过沉淀聚合合成分子印迹聚合物(MIP)的方法,以巴比妥作为模板分子,并将巴比妥 MIP 作为一种分子选择性吸附剂应用于从人尿样中固相萃取(SPE)巴比妥类药物。MIP 通过沉淀聚合,以 2,6-双丙烯酰胺吡啶为功能单体和 DVB-80 为交联剂合成。所制备的球形 MIP 颗粒的直径为 4.2±0.4μm;珠状的非印迹对照聚合物(NIP)的直径为 4.8±0.4μm(平均值±标准偏差)。将颗粒填充到固相萃取柱中,并作为一种新型吸附剂用于分子印迹固相萃取(MISPE)方案中。MIP 对模板分子巴比妥表现出高选择性,这一特性可归因于 2,6-双丙烯酰胺吡啶作为功能单体的使用,导致 MIP 中存在高保真结合位点。然而,MIP 对除巴比妥以外的其他巴比妥类药物也表现出有用的交叉选择性。对于实际样品,将 MIP 用于从人尿中提取四种巴比妥类药物。然而,由于该样品中高浓度的尿素会干扰巴比妥类药物与 MIP 的适当相互作用,因此开发了一种使用市售吸附剂的串联系统。