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基于选择性分子印迹聚合物的水样中吲哚美辛固相萃取方法的开发。

Development of a selective molecularly imprinted polymer-based solid-phase extraction for indomethacin from water samples.

作者信息

Yang Tao, Li Ya-Hui, Wei Shuang, Li Yuan, Deng Anping

机构信息

College of Chemistry, Sichuan University, Wangjiang Road 29, Chengdu, 610064, China.

出版信息

Anal Bioanal Chem. 2008 Aug;391(8):2905-14. doi: 10.1007/s00216-008-2218-2. Epub 2008 Jun 25.

Abstract

A selective molecularly imprinted solid-phase extraction (MISPE) for indomethacin (IDM) from water samples was developed. Using IDM as template molecule, acrylamide (AM) or methacrylic acid (MAA) as functional monomer, ethylene dimethacrylate (EDMA) as crosslinker, and bulk or suspension polymerization as the synthetic method, three molecularly imprinted polymers (MIPs) were synthesized and characterized with a rebinding experiment. It was found that the MIP of AM-EDMA produced by bulk polymerization showed the highest binding capacity for IDM, and so it was chosen for subsequent experiments, such as those testing the selectivity and recognition binding sites. Scatchard analysis revealed that at least two kinds of binding sites formed in the MIP, with the dissociation constants of 7.8 micromol L(-1) and 127.2 micromol L(-1), respectively. Besides IDM, three structurally related compounds--acemetacin, oxaprozin and ibuprofen--were employed for selectivity tests. It was observed that the MIP exhibited the highest selective rebinding to IDM. Accordingly, the MIP was used as a solid-phase extraction sorbent for the extraction and enrichment of IDM in water samples. The extraction conditions of the MISPE column for IDM were optimized to be: chloroform or water as loading solvent, chloroform with 20% acetonitrile as washing solution, and methanol as eluting solvent. Water samples with or without spiking were extracted by the MISPE column and analyzed by HPLC. No detectable IDM was observed in tap water and the content of IDM in a river water sample was found to be 1.8 ng mL(-1). The extraction efficiencies of the MISPE column for IDM in spiked tap and river water were acceptable (87.2% and 83.5%, respectively), demonstrating the feasibility of the prepared MIP for IDM extraction.

摘要

开发了一种从水样中选择性分离吲哚美辛(IDM)的分子印迹固相萃取(MISPE)方法。以IDM为模板分子,丙烯酰胺(AM)或甲基丙烯酸(MAA)为功能单体,乙二醇二甲基丙烯酸酯(EDMA)为交联剂,采用本体聚合或悬浮聚合法合成了三种分子印迹聚合物(MIP),并通过再结合实验对其进行了表征。结果发现,通过本体聚合制备的AM-EDMA-MIP对IDM的结合能力最高,因此被选用于后续实验,如选择性测试和识别结合位点测试。Scatchard分析表明,该MIP中至少形成了两种结合位点,其解离常数分别为7.8 μmol L⁻¹和127.2 μmol L⁻¹。除IDM外,还选用了三种结构相关的化合物——阿西美辛、恶丙嗪和布洛芬进行选择性测试。结果表明,该MIP对IDM表现出最高的选择性再结合能力。因此,该MIP被用作固相萃取吸附剂,用于水样中IDM的萃取和富集。优化了MISPE柱对IDM的萃取条件:以氯仿或水为上样溶剂,以含20%乙腈的氯仿为洗涤液,以甲醇为洗脱溶剂。采用MISPE柱对加标和未加标的水样进行萃取,并通过高效液相色谱法进行分析。自来水中未检测到IDM,河水样品中IDM的含量为1.8 ng mL⁻¹。MISPE柱对加标自来水和河水中IDM的萃取效率均可接受(分别为87.2%和83.5%),证明了所制备的MIP用于IDM萃取的可行性。

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