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采用分子印迹聚合物固相萃取和高效液相色谱法分离和测定水样中的雌激素。

Isolation and determination of estrogens in water samples by solid-phase extraction using molecularly imprinted polymers and HPLC.

机构信息

Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, Toruń, Poland.

出版信息

J Sep Sci. 2013 Jul;36(14):2299-305. doi: 10.1002/jssc.201300366. Epub 2013 Jun 21.

Abstract

Advanced SPE with molecularly imprinted polymers (MIP) was used in this study. A noncovalent imprinting approach was applied to separate 17β-estradiol, estriol, and estrone from water samples. Polymer material was prepared by bulk polymerization with methacrylic acid as a functional monomer, divinylbenzene and ethyleneglycol dimethacrylate as crosslinkers, and acetonitrile, acetonitrile/toluene (3:1, v/v) or isooctane/toluene (1:99, v/v) as a porogen. We also prepared an MIP film on a silica gel surface with methacrylic acid and ethyleneglycol dimethacrylate as monomers and acetonitrile as a solvent. Qualitative and quantitative hormone analyses were carried out by HPLC with various detection techniques, including UV/visible spectroscopic detection (diode array detection) and electrochemical detection (CoulArray). The results of the study indicate that MIP technology is an excellent method for the quality control of estrogens in environmental analyses with a low quantification limit for 17β-estradiol of around 26 (diode array detection) and 0.25 ng/mL (electrochemical detection). The proposed method was found to be suitable for routine determinations of the analyzed compound in environmental laboratories.

摘要

本研究采用了高级固相萃取(SPE)与分子印迹聚合物(MIP)。应用非共价印迹方法从水样中分离 17β-雌二醇、雌三醇和雌酮。聚合材料通过本体聚合制备,以甲基丙烯酸为功能单体、二乙烯基苯和乙二醇二甲基丙烯酸酯为交联剂,乙腈、乙腈/甲苯(3:1,v/v)或异辛烷/甲苯(1:99,v/v)为致孔剂。我们还在硅胶表面上用甲基丙烯酸和乙二醇二甲基丙烯酸酯作为单体,乙腈作为溶剂制备了 MIP 膜。采用 HPLC 结合各种检测技术,包括紫外/可见光谱检测(二极管阵列检测)和电化学检测(库仑阵列检测)进行定性和定量激素分析。研究结果表明,MIP 技术是环境分析中雌激素质量控制的一种极好方法,17β-雌二醇的定量限低至约 26(二极管阵列检测)和 0.25ng/mL(电化学检测)。该方法适用于环境实验室中分析物的常规测定。

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