Microwave-assisted preparation of monolithic molecularly imprinted polymeric fibers for solid phase microextraction.
Microwave-assisted preparation of monolithic molecularly imprinted polymeric fibers for solid phase microextraction.
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DOI：
10.1039/c3an00003f
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发表时间：
2013-04
期刊：
影响因子：
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通讯作者：
Shuxia Xu;Xinfeng Zhang;Yonghua Sun;D. Yu
中科院分区：
文献类型：
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作者：
Shuxia Xu;Xinfeng Zhang;Yonghua Sun;D. Yu
本文提出了一种新的微波辅助快速批量制备整体式分子印迹聚合物（MIP）纤维的方法。它是基于在微波辐射下的柔性毛细管模具中的原位聚合。该方法大大缩短了制备时间（约20倍）相比，传统的加热。以双酚A（BPA）为模板分子，制备了印迹MIP纤维，并将其用于固相微萃取（SPME），然后用高效液相色谱（HPLC）测定BPA及其类似物，己烯雌酚（DES）和己雌酚（HEX）。在最佳条件下，BPA、DES和HEX的检出限分别为2.0 ng mL（-1）、5.1 ng mL（-1）和3.3 ng mL（-1）。纤维间提取（n = 5）具有重现性，相对标准偏差在6.6- 9.5%范围内。用MIP纤维对自来水、污水和尿样中的BPA、DES和HEX进行选择性萃取，MIP-SPME-HPLC法测定BPA、DES和HEX的相对回收率为82.5%~ 103.8%。这种微波辅助的方法所提供的优点将使其成为一个有用的工具，制备具有良好的SPME性能的MIP纤维。
In this work, a novel microwave-assisted method was developed for fast and batch fabrication of monolithic molecularly imprinted polymer (MIP) fibers. It was based on in situ polymerization in a flexible capillary mold under microwave irradiation. The proposed method greatly shortened the preparation time (about 20-fold) in comparison with the conventional heating. The model template, bisphenol A (BPA) imprinted MIP fiber, was prepared and used for solid phase microextraction (SPME) prior to high performance liquid chromatography (HPLC) determination of BPA and its analogues, i.e., diethylstilbestrol (DES) and hexestrol (HEX). Under the established optimum conditions, the limits of detection for BPA, DES and HEX were 2.0 ng mL(-1), 5.1 ng mL(-1), and 3.3 ng mL(-1), respectively. The fiber-to-fiber extraction (n = 5) was reproducible with the relative standard deviation in the range of 6.6-9.5%. The MIP fiber was used for selective extraction of BPA, DES and HEX in tap water, sewage and urine samples, and the relative recoveries for MIP-SPME-HPLC analysis of BPA, DES and HEX ranged from 82.5% to 103.8%. The advantages provided by this microwave-assisted method will make it a useful tool for preparation of MIP fibers with good SPME performance.