A new strategy for synthesis of an in-tube molecularly imprinted polymer-solid phase microextraction device: selective off-line extraction of 4-nitrophenol as an example of priority pollutants from environmental water samples

Anal Chim Acta. 2013 Oct 10:798:48-55. doi: 10.1016/j.aca.2013.08.038. Epub 2013 Sep 4.

Abstract

In this study a novel preparation protocol has been developed for the construction of an in-tube molecularly imprinted polymer-solid phase microextraction (MIP-SPME) device. Open tubular capillaries have been molded from a polymer sorbent imprinted for 4-nitrophenol as target molecule. Different parameters like inner diameter and volume of the polymer, porogen volume, swelling and shrinking effects of the polymer tubes, polymerization time, pH of the sample, extraction time, 'salting out' effect and serial connection of the tubes were evaluated and optimized. Particularly, an optimized polymer preparation process and extraction condition enhanced the final extraction recovery of 4-nitrophenol substantially. Using this new MIP-SPME technique with high-performance liquid chromatography-ultraviolet (HPLC-UV) analysis of the extracts, the linear range and the limits of detection and quantification are 0.001-10 mg L(-1), 0.33 μg L(-1) and 1.1 μg L(-1) respectively. At optimized conditions, a mixture of nitrophenols, alkylated and chlorinated phenols spiked into municipal waste water were analyzed to evaluate the matrix effects and cross selectivity of the new MIP capillary tubes.

Keywords: 4-nitrophenol; In-tube; Molecularly imprinted polymer; Solid phase microextraction.