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Quantification of 10,11-dihydro-10-hydroxy carbamazepine and 10,11-epoxycarbamazepine as the main by-products in the electrochemical degradation of carbamazepine

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Abstract

Carbamazepine (CBZ) is one of the most widely used antiepileptic drugs in Malaysia. It was detected frequently in wastewater. The electrochemical treatment process has been applied for the degradation of CBZ using graphite–PVC as an anode under these conditions: 0.5 g sodium chloride (NaCl)) as supporting electrolyte, 5 V and 0–60 min electrolysis time in 100 mL of solution. However, 10,11-dihydro10-hydroxy carbamazepine (HDX-CBZ) and 10,11-epoxycarbamazepine (EPX-CBZ) as the main by-product have been analysed and quantified using liquid chromatography–time of flight/mass spectrometry (LC-TOF/MS). Both by-products were analysed in positive ionization mode, and they were separated on a chromatographic C18 column (5 μm, 2 mm × 150 mm) at a flow rate of 0.3 mL/min. Solid-phase extraction (SPE) was applied as a pre-concentration step for the enhancement of the sensitivity and detectability for both HDX-CBZ and EPX-CBZ by-products. Methanol (MeOH) has been selected as the best elution solvent for both by-products compared to methyl tertiary butyl ether (MTBE) and acetone (AC). However, the recovery was 85% and 92% for HDX-CBZ and EPX-CBZ by-products, respectively. The limit of quantification (LOQ) was 0.588 and 0.109 µg/L for HDX-CBZ and EPX-CBZ by-products, respectively. After 20 min of electrolysis time, both by-products HDX-CBZ and EPX-CBZ appeared at maximum concentrations of 343 and 144 μg/L then they were decreased to 17.2 and 9.8 μg/L, respectively, after 40 min. At the end of electrochemical treatment, both by-products were completely eliminated after 60 min.

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Acknowledgements

Support for this study was provided by the Central Research Instrumentation of Management, Universiti Kebangsaan Malaysia. The authors would like to thank all staff in the centre.

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Authors and Affiliations

  1. College of Pharmacy, University of Al-Ameed, Kerbala, Iraq

    Zainab Haider Mussa

  2. Malaysia-Japan International Institute of Technology (MJIIT), Universiti Teknologi Malaysia, Jalan Sultan Yahya Petra, 54100, Kuala Lumpur, Malaysia

    Zainab Haider Mussa & Fouad Fadhil Al-Qaim

  3. Department of Chemistry, College of Science for Women, University of Babylon, Hillah, Iraq

    Fouad Fadhil Al-Qaim

Authors
  1. Zainab Haider Mussa
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  2. Fouad Fadhil Al-Qaim
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Contributions

Zainab Haider Mussa: lab work, methodology, data collection, electrochemical cell construction.

Fouad Fadhil Al-Qaim: methodology, validation, writing (original draft), writing (editing), elucidation the by-products.

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Correspondence to Fouad Fadhil Al-Qaim.

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Mussa, Z.H., Al-Qaim, F.F. Quantification of 10,11-dihydro-10-hydroxy carbamazepine and 10,11-epoxycarbamazepine as the main by-products in the electrochemical degradation of carbamazepine. Environ Sci Pollut Res 29, 62447–62457 (2022). https://doi.org/10.1007/s11356-022-20091-7

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  • DOI: https://doi.org/10.1007/s11356-022-20091-7

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