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分子印迹固相萃取-高效液相色谱法选择性测定渔业样品中的17β-雌二醇

Molecularly imprinted solid-phase extraction for the selective determination of 17beta-estradiol in fishery samples with high performance liquid chromatography.

作者信息

Jiang Tianhe, Zhao Lixia, Chu Baolin, Feng Qinzhong, Yan Wei, Lin Jin-Ming

机构信息

State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China.

出版信息

Talanta. 2009 Apr 30;78(2):442-7. doi: 10.1016/j.talanta.2008.11.047. Epub 2008 Dec 9.

Abstract

A molecularly imprinted polymer (MIP) has been synthesized by a thermo-polymerization method using methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross-linker, acetonitrile as porogenic solvent, and 17beta-estradiol as template. The MIP showed obvious affinity for 17beta-estradiol in acetonitrile solution, which was confirmed by absorption experiments. After optimization of molecularly imprinted solid-phase extraction (MISPE) conditions, three structurally related estrogenic compounds (17beta-estradiol, estriol, and diethylstilbestrol) were used to evaluate the selectivity of the MIP cartridges. The MIP cartridges exhibited highly selectivity for E(2), the recoveries were 84.8+/-6.53% for MIPs and 19.1+/-1.93% for non-imprinted polymer (NIP) cartridges. The detection and quantification limits correspond to 0.023 and 0.076 mg L(-1). Furthermore, the MISPE methods were used to selectively extract E(2) from fish and prawn tissue prior to HPLC analysis. This MISPE-HPLC procedure could eliminate all matrix interference simultaneously and had good recoveries (78.3-84.5%).

摘要

采用热聚合方法,以甲基丙烯酸(MAA)为功能单体、乙二醇二甲基丙烯酸酯(EGDMA)为交联剂、乙腈为致孔溶剂、17β-雌二醇为模板,合成了一种分子印迹聚合物(MIP)。吸收实验证实,该MIP在乙腈溶液中对17β-雌二醇表现出明显的亲和力。在优化分子印迹固相萃取(MISPE)条件后,使用三种结构相关的雌激素化合物(17β-雌二醇、雌三醇和己烯雌酚)评估MIP柱的选择性。MIP柱对E(2)表现出高度选择性,MIP柱的回收率为84.8±6.53%,非印迹聚合物(NIP)柱的回收率为19.1±1.93%。检测限和定量限分别为0.023和0.076 mg L(-1)。此外,在进行HPLC分析之前,采用MISPE方法从鱼和虾组织中选择性提取E(2)。这种MISPE-HPLC方法可以同时消除所有基质干扰,回收率良好(78.3-84.5%)。

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