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Extraction Strategies for Simultaneous Determination of Florfenicol and Florfenicol Amine in Tilapia (Oreochromis niloticus) Muscle: Quantification by LC-MS/MS

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Abstract

A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of the veterinary drug florfenicol (FF) and its major metabolite, florfenicol amine (FFA), in tilapia muscles (Oreochromis niloticus). Three different sample preparation procedures (DLLME, sub-zero, and modified QuEChERS) were tested. The best extraction results were obtained by using the modified QuEChERS. The quantification was made by using a LC-MS/MS analysis, with a Lichrocart Cartridge Purospher Star C8 HPLC column (250 mm×4.6 mm, 5 μm particle size). Analytes were separated with a mobile phase consisting of Milli-Q water to acetonitrile 40:60 (v/v), both with 0.1% formic acid. The validation parameters were recovery of 70 to 79% and 62 to 69%, limit of detection of 0.0625 μg g−1 and 0.125 μg g−1, and limit of quantification of 0.125 μg g−1 and 0.25 μg g−1, for FF and FFA, respectively. CCα was 1183 μg kg−1 and CCβ was 1365 μg kg−1 for FF, intraday and interday precision has CV ≤20%, and linear range was 0.625 to 5.00 μg g−1. This method was shown to be simple and rapid when compared to other, more conventional methods. Also, it has low reagent and solvent consumption, with low waste generation, which is in line with the principles of green chemistry. The method was successfully applied for the analyzes of tilapia exposed to the antibiotic.

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Abbreviations

CCα :

Limit of decision

CCβ :

Detection capacity

EC:

European Commission

FF:

Florfenicol

FFA:

Florfenicol amine

MAPA:

Ministry of Agriculture, Livestock and Food Supply - Brazil

MISPE:

Molecularly imprinted solid-phase extraction

MSPD:

Matrix solid-phase dispersion extraction

QuEChERS:

Quick, Easy, Cheap, Effective, Rugged and Safe

UA-DLLME:

Ultrasound-assisted dispersive liquid-liquid microextraction

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Acknowledgments

The authors wish to thank Prof. Carol Collins for language assistance.

Funding

This research was supported by BNDES (0117020010606007), FAPESP (2014/50867-3), CNPq (311671/2015-2; 465389/2014-7) and INCT Bioanalítica. This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), Brazil, Finance Code 001.

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Authors and Affiliations

  1. Institute of Chemistry, University of Campinas, POB 6154, Campinas, SP, 13083-970, Brazil

    Letícia Sayuri Shiroma & Carla Beatriz Grespan Bottoli

  2. Laboratory of Residues and Contaminants, Embrapa Meio Ambiente, Rodovia SP 340, km 127,5, S/N, Jaguariuna, SP, 13918-110, Brazil

    Sonia C. N. Queiroz & Claudio Martin Jonsson

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  1. Letícia Sayuri Shiroma
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  2. Sonia C. N. Queiroz
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  3. Claudio Martin Jonsson
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  4. Carla Beatriz Grespan Bottoli
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Correspondence to Carla Beatriz Grespan Bottoli.

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Letícia Sayuri Shiroma, Sonia Claudia do Nascimento de Queiroz, Claudio Martin Jonsson and Carla Beatriz Grespan Bottoli declare no conflict of interest.

Ethical Approval

This article contains studies with animals approved by Ethical Commission for the Use of Animals (CEUA) of the Embrapa Environment (Registration 007/17) (Jonsson et al. 2017).

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Shiroma, L.S., Queiroz, S.C.N., Jonsson, C.M. et al. Extraction Strategies for Simultaneous Determination of Florfenicol and Florfenicol Amine in Tilapia (Oreochromis niloticus) Muscle: Quantification by LC-MS/MS. Food Anal. Methods 13, 291–302 (2020). https://doi.org/10.1007/s12161-019-01633-1

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