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HPLC–DAD–FLD Determination of Veterinary Pharmaceuticals in Pharmaceutical Industry Wastewater with Precolumn Derivatization Using Fluorescamine

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Abstract

A simple and robust method suitable for routine analysis of pharmaceuticals from different classes in pharmaceutical industry wastewater samples is presented. Seven veterinary pharmaceuticals (antibiotics and anesthetic) were simultaneously isolated from a highly complex wastewater matrix. Target compounds were three sulfonamide antibiotics (sulfaguanidine, sulfadiazine, and sulfamethazine), three fluoroquinolone antibiotics (ciprofloxacin, enrofloxacin, norfloxacin), and one anesthetic, procaine. The investigated compounds were simultaneously pre-concentrated and cleaned up by solid-phase extraction using Strata-X extraction cartridges. The analysis was performed using liquid chromatography (LC) with diode array and fluorescence detectors connected in series to the chromatographic system. LC separation was performed on a C18 modified column (Phenomenex) with a gradient elution of mobile phase (0.1 % acetic acid in water and 0.1 % acetic acid in acetonitrile) in 25 min at 30 °C. Recoveries ranged from 86.9 to 110 % with relative standard deviations below 10.1 %. Method limits of quantification were in the range of 0.005–0.1 μg L−1 depending on the fluorescence intensity after precolumn derivatization by fluorescamine.

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Acknowledgments

This work was supported by the Croatian Ministry of Science, Education, and Sports Project: 125-1253008-1350, Development of advanced analytical methods for pharmaceuticals determination in the environment, and a bilateral project HR-SLO: Determination of toxicity and physico-chemical properties of pharmaceuticals.

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 20, 10000, Zagreb, Croatia

    Danijela Ašperger, Vesna Tišler, Mirta Zrnčić, Dragana Mutavdžić Pavlović, Sandra Babić, Alka J. M. Horvat & Marija Kaštelan-Macan

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  1. Danijela Ašperger
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  2. Vesna Tišler
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  3. Mirta Zrnčić
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  4. Dragana Mutavdžić Pavlović
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  5. Sandra Babić
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  6. Alka J. M. Horvat
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  7. Marija Kaštelan-Macan
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Corresponding author

Correspondence to Danijela Ašperger.

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Published in the special paper collection 19th International Symposium on Separation Sciences with guest editors Tomislav Bolanča and Bogusław Buszewski.

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Ašperger, D., Tišler, V., Zrnčić, M. et al. HPLC–DAD–FLD Determination of Veterinary Pharmaceuticals in Pharmaceutical Industry Wastewater with Precolumn Derivatization Using Fluorescamine. Chromatographia 77, 1059–1066 (2014). https://doi.org/10.1007/s10337-014-2685-x

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  • DOI: https://doi.org/10.1007/s10337-014-2685-x

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