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Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS)

Analytical and Bioanalytical Chemistry volume 398, pages 1185–1194 (2010)Cite this article

Abstract

An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography–tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L−1 in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.

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Acknowledgements

This work was supported by the Unity Through Knowledge Fund (UKF), which was established by the Croatian Ministry of Science, Education and Sports through World Bank Loan No. 7320-HR: Reduction of environmental risks posed by pharmaceuticals and their degradation products in process wastewaters, through RO/NF membrane treatment (REPHAD), and Croatian Ministry of Science, Education and Sports Projects: 125-1253008-1350 and 125-2120898-3148.

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  1. Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, 10000, Zagreb, Croatia

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

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  1. Sandra Babić
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  2. Dragana Mutavdžić Pavlović
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  3. Danijela Ašperger
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  4. Martina Periša
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  5. Mirta Zrnčić
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  6. Alka J. M. Horvat
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  7. Marija Kaštelan-Macan
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Correspondence to Sandra Babić.

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Babić, S., Mutavdžić Pavlović, D., Ašperger, D. et al. Determination of multi-class pharmaceuticals in wastewater by liquid chromatography–tandem mass spectrometry (LC–MS–MS). Anal Bioanal Chem 398, 1185–1194 (2010). https://doi.org/10.1007/s00216-010-4004-1

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  • DOI: https://doi.org/10.1007/s00216-010-4004-1

Keywords

  • Pharmaceuticals
  • Wastewater
  • Liquid chromatography–tandem mass spectrometry
  • Solid phase extraction