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Hexafluoroisopropanol-mediated cloud point extraction of organic pollutants in water with analysis by high-performance liquid chromatography

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Abstract

A hexafluoroisopropanol (HFIP)-mediated cloud point extraction (CPE) system was established. A small amount of HFIP (even 1%, v/v) can dramatically reduce the cloud point of Triton X-100 (TX-100) aqueous solution (even to 1 °C) and make liquid-liquid two-phase separation (coacervate phase and aqueous phase) occur at room temperature over a wide range of TX-100 concentration (0.5∼10%, g/mL). HFIP-mediated coacervate phase has smaller volume (volume ratio is 1.8∼8.9% relative to the volume of the total solution with 1∼5% TX-100) and larger micelle aggregates (30∼80 nm in diameter) compared to temperature-induced coacervate phase (volume ratio at 2.8∼14.0%, the diameter of micelle aggregates at 5∼30 nm). HFIP-mediated CPE was coupled to high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the extraction and detection of organic pollutants in water, namely, polycyclic aromatic hydrocarbons (PAHs), fluoroquinolones (FQs), and sulfonamides (SAs) with different polarities, charges, and hydrogen-bonding properties. HFIP-mediated CPE provides much higher extraction rates (ERs) and enrichment factors (EFs) for FQs (91∼106%, 50∼59), PAHs (63∼90%, 33∼49), and SAs (26∼55%, 16∼34) compared with the temperature-induced one (ERs: 4∼8% for FQs, 25∼46% for PAHs, and 4∼37% for SAs; EFs: 1∼3 for FQs, 6∼12 for PAHs, and 8∼13 for SAs). The limit of detection ranges from 0.24 to 0.33 ng/mL for FQs, 0.04 to 0.38 ng/mL for PAHs, and 0.63 to 1.31 ng/mL for SAs. The proposed method was applied in the analysis of real water samples, and the recovery of 79.4∼110.8% and the relative standard deviation of 0.2∼16.3% were achieved for the three types of pollutants.

Schematic illustration of HFIP-mediated cloud point extraction

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Acknowledgements

A fluorescent dye called BODIPY was kindly provided by Prof. Xuechuan Hong in Wuhan University School of Pharmaceutical Sciences. We thank the National Natural Science Foundation of China (Grant nos. 81373045 and 81673394), the Provincial Natural Science Foundation of Hubei of China (Grant no. 2015CFA139), and the Innovation Seed Fund of Wuhan University School of Medicine (Grant no. 266078).

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Authors and Affiliations

  1. Key Laboratory of Combinatorial Biosynthesis and Drug Discovery (Ministry of Education), and School of Pharmaceutical Sciences, Wuhan University, 185 Donghu Road, Wuchang District, Wuhan, Hubei, 430071, China

    Jia Xu, Yunfang Li, Cao Li, Rui Zhang & Yuxiu Xiao

  2. College of Pharmacy, South Central University for Nationalities, Hongshan District, Wuhan, Hubei, 430074, China

    Yunfang Li

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  1. Jia Xu
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Correspondence to Yuxiu Xiao.

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Xu, J., Li, Y., Li, C. et al. Hexafluoroisopropanol-mediated cloud point extraction of organic pollutants in water with analysis by high-performance liquid chromatography. Anal Bioanal Chem 409, 4559–4569 (2017). https://doi.org/10.1007/s00216-017-0394-7

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  • DOI: https://doi.org/10.1007/s00216-017-0394-7

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