Evaluation of a Selective Approach for the Determination of 5-Nitroimidazoles in Aquaculture Products by Capillary Liquid Chromatography Using Molecularly Imprinted Solid-Phase Extraction

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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Corresponding author

Correspondence to Ana M. García-Campaña.

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Funding

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.

Conflict of Interest

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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Keywords

  • 5-Nitroimidazoles
  • Aquaculture products
  • Capillary liquid chromatography
  • Molecularly imprinted solid-phase extraction