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Salt-induced ionic liquid-based microextraction using a low cytotoxic guanidinium ionic liquid and liquid chromatography with fluorescence detection to determine monohydroxylated polycyclic aromatic hydrocarbons in urine

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Abstract

A novel ionic liquid (IL)-based microextraction method has been developed for the determination of four hydroxylated polycyclic aromatic hydrocarbons (OHPAHs) in urine samples. The water soluble IL-based surfactant selected as extraction solvent is decylguanidinium chloride (C10Gu-Cl), the cytotoxicity and micellar behavior of which were evaluated. The proposed salt-induced IL-based preconcentration method simply consists in adding NaClO4 to the aqueous medium containing the IL to promote its water insolubility. The entire method was optimized, requiring the use of only 20 μL of C10Gu-Cl for 10 mL of diluted urine sample (1:10) without any pH adjustment, followed by the addition of NaClO4 to ensure a 5% (w/v) content. A cloudy solution was observed immediately, and after the application of 4 min of vortex and 8 min of centrifugation, the droplet was diluted up to 60 μL with a mixture of acetonitrile:water (30:70) and injected into the liquid chromatograph with fluorescence detection. The method was validated using both synthetic urine and human urine as matrix for the determination of the four OHPAHs. The following analytical features were obtained: detection limits down to 1 ng·L-1 in real urine; inter-day reproducibility (as RSD in %) always lower than 17% when dealing with real urine samples spiked at 80 ng·L-1; and average relative recoveries of 102% in real urine samples at such low spiked levels. Despite the simplicity of the proposed method, it performed successfully with complex urine samples.

Salt-induced IL-based microextraction using a low cytotoxic IL for mono-OHPAHs in urine

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Acknowledgements

I.P.-F. is thankful for her PhD research contract from ULL-La Caixa fellowship. V.P. thanks the Spanish Ministry of Economy and Competitiveness (MINECO) for the project MAT2014-57465-R. J.L.-M. acknowledges the grant “Red de Investigation Colaborativa en Enfermedades Tropicales” RICET (project RD16/0027/0001 of the program of “Redes Temáticas de Investigación Cooperativa”, FIS, Spanish Ministry of Health) and “Ayudas Plan Propio de la Universidad de La Laguna 2017 (proyectos puente I+D+i)”.

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Authors and Affiliations

  1. Departamento de Química, UD de Química Analítica, Universidad de La Laguna (ULL), 38206 La Laguna, Tenerife, Spain

    Idaira Pacheco-Fernández, Verónica Pino, Juan H. Ayala & Ana M. Afonso

  2. University Institute of Tropical Diseases and Public Health, Universidad de La Laguna (ULL), 38206 La Laguna, Tenerife, Spain

    Jacob Lorenzo-Morales

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  1. Idaira Pacheco-Fernández
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  2. Verónica Pino
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  3. Jacob Lorenzo-Morales
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  4. Juan H. Ayala
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  5. Ana M. Afonso
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Corresponding author

Correspondence to Verónica Pino.

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Volunteers signed an individual informed consent in order to use their urine samples in this study. This study was approved by the Universidad de La Laguna ethical committee and has been performed in accordance with Spanish ethical standards in research.

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The authors declare that they have no conflict of interest.

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Published in the topical collection Ionic Liquids as Tunable Materials in (Bio)Analytical Chemistry with guest editors Jared L. Anderson and Kevin D. Clark.

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Pacheco-Fernández, I., Pino, V., Lorenzo-Morales, J. et al. Salt-induced ionic liquid-based microextraction using a low cytotoxic guanidinium ionic liquid and liquid chromatography with fluorescence detection to determine monohydroxylated polycyclic aromatic hydrocarbons in urine. Anal Bioanal Chem 410, 4701–4713 (2018). https://doi.org/10.1007/s00216-018-0946-5

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