Abstract
Capillary liquid chromatography with UV detection is proposed for the determination of 5-nitroimidazole residues in aquaculture products. The separation was carried out in a C18 column at 20 °C, using a mobile phase consisting of water and acetonitrile, at 7 μL/min and 320 nm as detection wavelength. Furthermore, full loop injection mode (8 μL) was selected and water was considered as injection solvent. The optimized method was applied to the monitoring of nine 5-nitroimidazoles, including three metabolites, in crab, salmon, prawn, and velvet swimming crab. Molecularly imprinted solid-phase extraction has been evaluated for sample cleanup. The method was characterized in all the matrices in terms of linearity (R 2 ≥ 0.9964), precision (repeatability, RSD ≤ 7.9%, and reproducibility, RSD ≤ 11.1%) and trueness (recoveries between 80.4 and 108.7%). Decision limits, CCα, ranging from 0.2 to 1.5 μg/kg and detection capabilities, CCβ, from 0.2 to 1.8 μg/kg, were obtained.
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Abbreviations
- CCβ:
-
Detection capability
- CCα:
-
Decision limit
- DMZ:
-
Dimetridazole
- EURLs:
-
European Union Reference Laboratories
- HMMNI:
-
2-Hydroxymethyl-1-methyl-5-nitro-1H-imidazole
- IPZ:
-
Ipronidazole
- IPZ-OH:
-
Hydroxyl-ipronidazole
- MISPE:
-
Molecularly imprinted solid-phase extraction
- MNZ:
-
Metronidazole
- MNZ-OH:
-
Hydroxyl-metronidazole
- MRLs:
-
Maximum residue levels
- 5-NDZ:
-
5-Nitroimidazole
- ORZ:
-
Ornidazole
- RNZ:
-
Ronidazole
- SCZ:
-
Secnidazole
- SPE:
-
Solid-phase extraction
- TNZ:
-
Tinidazole
- TRZ:
-
Ternidazole
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This study was funded by the Andalusian Government (Junta de Andalucía) for Excellence Project Ref: P12-AGR-1647. M. Hernández-Mesa thanks the “Plan Propio” of University of Granada for a pre-doctoral fellowship. D. Moreno-González acknowledges the program to strengthen research groups of the University of Granada for his postdoctoral contract.
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M. Hernández-Mesa declares that he has no conflict of interest. D. Moreno-González declares that he has no conflict of interest. C. Cruces-Blanco declares that she has no conflict of interest. A.M. García-Campaña declares that she has no conflict of interest.
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This article does not contain any studies with human participants or animals performed by any of the authors.
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Hernández-Mesa, M., Moreno-González, D., Cruces-Blanco, C. et al. Evaluation of a Selective Approach for the Determination of 5-Nitroimidazoles in Aquaculture Products by Capillary Liquid Chromatography Using Molecularly Imprinted Solid-Phase Extraction. Food Anal. Methods 10, 3647–3657 (2017). https://doi.org/10.1007/s12161-017-0928-9
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DOI: https://doi.org/10.1007/s12161-017-0928-9