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New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC

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Abstract

A novel porous monolith has been prepared and used as a sorbent in stir-cake-sorptive extraction (SCSE). The monolithic material was prepared by in-situ copolymerization of allyl thiourea (AT) and divinylbenzene (DB) in the presence of dimethylformamide as a porogen solvent. To optimize the polymerization conditions, different monoliths with different ratios of functional monomer to porogenic solvent were prepared, and their extraction efficiency was investigated in detail. The monolith was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, and infrared spectroscopy. Analysis of polar phenols in environmental water samples by a combination of ATDB-SCSE and HPLC with diode-array detection was selected as a model for the practical application of the new sorbent. Several extraction conditions, including extraction and desorption time, pH, and ionic strength of the sample matrix were optimized. The results showed that the new monolith had high affinity for polar phenols and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the phenols, within the ranges 0.18–0.90 and 0.59–2.97 μg L−1, respectively. The linearity of the method was good, and the method enabled simple, practical, and low-cost extraction of these analytes. The distribution coefficients between ATDB and water (K ATDB/W) were calculated for the phenolic compounds and compared with K O/W. Finally, the proposed method was successfully applied to the determination of the compounds in three environmental water samples, with acceptable recovery and satisfactory repeatability.

HPLC chromatograms of real water sample treated with ATDB-SCSE (a) and spiked water sample treated with ATDB-SCSE (b)

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Acknowledgements

Dr XJ Huang is grateful for support from the National Natural Science Foundation of China (grant 21077085), the Scientific Research Foundation for Returned Overseas Chinese Scholars, the State Education Ministry, the New Century Excellent Talents in Fujian Province University, and Fundamental Research Funds for Central Universities (no. CXB2011037). Dr XJ Li is grateful for support from the Fujian Provincial Key Program of Science and Technology (no. 2011Y0001).

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Authors and Affiliations

  1. State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, P.O. Box 1009, Xiamen, 361005, China

    Xiaojia Huang, Yulei Wang, Dongxing Yuan & Shuyu Nong

  2. Technique Center of Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou, 350001, China

    Xiaojing Li

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  1. Xiaojia Huang
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  2. Yulei Wang
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  3. Dongxing Yuan
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  4. Xiaojing Li
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  5. Shuyu Nong
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Correspondence to Xiaojia Huang.

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Published in the topical collection Monolithic Columns in Liquid Phase Separations with guest editor Luis A. Colon.

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Huang, X., Wang, Y., Yuan, D. et al. New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC. Anal Bioanal Chem 405, 2185–2193 (2013). https://doi.org/10.1007/s00216-012-6301-3

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  • DOI: https://doi.org/10.1007/s00216-012-6301-3

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