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Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed

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Abstract

In conventional microextraction procedures, the disperser (organic solvent or ionic liquid) is left in the aqueous phase and discarded after finishing the microextraction process. Because the disperser is water-soluble, it results in low extraction recovery for polar compounds. In this investigation, an ionic-liquid-based microextraction (ILBME) was integrated with salting-out assisted liquid-liquid microextraction (SALLME) to build an ionic-liquid-based, salt-induced, dual microextraction (ILSDME) for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P, −1.0 to 1.0). The proposed ILSDME method incorporates a dual microextraction by converting the disperser in the ILBME to the extractor in the SALLME. Optimization of key factors was conducted by integrating single-factor experiments and central composite design. The optimized experimental parameters were 80 μL [C8MIM][PF6] as extractor, 505 μL acetone as disperser, pH = 2.0, 4.1 min extraction time, and 4.2 g of Na2SO4. Under optimized conditions, high ERs (90.6–103.2 %) and low LODs (0.07–0.61 μg kg−1) were determined for five FQs in swine feed. Experimental precision based on RSDs was 1.4–5.2 % for intra-day and 2.4–6.9 % for inter-day analyses. The combination of ILBME with SALLME increased FQ recoveries by 15–20 % as compared with SALLME, demonstrating that the ILSDME method can enhance extraction efficiency for polar compounds compared to single-step microextraction. Therefore, the ILSDME method developed in this study has wide application for pretreatment of moderately to highly polar pollutants in complex matrices.

A dual microextraction was developed by integrating ionic-liquid-based microextraction with salting-out assisted liquid-liquid microextraction for isolation of five fluoroquinolone antibiotics (FQs) with high polarity (log P = −1.0 to 1.0). The principle of dual microextraction is based on converting the remaining disperser from the first microextraction into an extractor in the second microextraction. Single-factor experiment and central composite design were applied for optimizing operational parameters using 3D response surfaces and contour lines. Under optimized conditions, the method provided high extraction recoveries and low LODs for five FQs in swine feed. The prominent advantage of the dual microextraction is rapid and highly efficient extraction of moderately to highly polar fluoroquinolones from complex matrices

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Acknowledgments

This work was jointly supported by the China National Natural Science Foundation (21577107), the Zhejiang Provincial Public Benefit Project (2016C37019 and 2016C34011), the Zhejiang Provincial Natural Science Foundation (LY15B070009 and LY15B070010), and the Wenzhou International Cooperation Project (H20140004). The authors thank Professor Randy A. Dahlgren, employed in Davis, University of California, USA, for correcting this manuscript.

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    Authors and Affiliations

    1. College of Life Sciences, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China

      Huili Wang

    2. College of Marine Life, Ocean University of China, Qingdao, Shandong, 266000, China

      Ming Gao

    3. Key Laboratory of Watershed Sciences and Health of Zhejiang Province, Wenzhou Medical University, Wenzhou, Zhejiang, 325035, China

      Jiajia Gao, Nana Yu, Hong Huang, Qing Yu & Xuedong Wang

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    1. Huili Wang
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    Huili Wang and Ming Gao contributed equally to this work.

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    Wang, H., Gao, M., Gao, J. et al. Determination of fluoroquinolone antibiotics via ionic-liquid-based, salt-induced, dual microextraction in swine feed. Anal Bioanal Chem 408, 6105–6114 (2016). https://doi.org/10.1007/s00216-016-9719-1

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