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Simultaneous determination of malachite green, enrofloxacin and ciprofloxacin in fish farming water and fish feed by liquid chromatography with solid-phase extraction

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Abstract

An effective and sensitive method for simultaneous analysis of malachite green (MG), enrofloxacin (ENFLX) and ciprofloxacin (CPFLX) by liquid chromatography-diode array detection with solid-phase extraction (SPE) is developed. The conditions of SPE and LC were investigated and optimised. The effective separation of these compounds was achieved using a ZY1104 C18 column (250 × 4.6 mm, 5 μm) with 20 mM tetrabutyl ammonium bromide (pH  3.0)–acetonitrile as mobile phase and gradient elution. The diode array detection was used at 278 nm for ENFLX and CPFLX and at 613 nm for MG. Under the optimal conditions, the method LOD values of MG, ENFLX and CPFLX were 0.01, 0.07 and 0.10 μg L − 1 for fish farming water samples and 1.5, 10.5 and 15 μg kg − 1 for fish feed samples, respectively. The relative recoveries of the three analytes were achieved to be 76.7–82.3% with the RSDs (n = 5) of 3.2–4.6% for spiked fish farming water samples and 78.8–93.7% with the RSDs (n = 5) of 3.1–4.8% for spiked fish feed samples.

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References

  • Barrón, D., Jiménez-Lozano, E., Cano, J., & Barbosa, J. (2001). Determination of residues of enrofloxacin and its metabolite ciprofloxacin in biological materials by capillary electrophoresis. Journal of Chromatography B, 759, 73–79.

    Article  Google Scholar 

  • Bergwerff, A. A., & Scherpenisse, P. (2003). Determination of residues of malachite green in aquatic animals. Journal of Chromatography B, 788, 351–359.

    Article  CAS  Google Scholar 

  • Bose, B., Motiwale, L., & Rao, K. V. K. (2005). DNA damage and G2/M arrest in Syrian hamster embryo cells during Malachite green exposure are associated with elevated phosphorylation of ERK1 and JNK1. Cancer Letter, 230, 260–270.

    Article  CAS  Google Scholar 

  • Cinquina, A. L., Roberti, P., Giannetti, L., Longo, F., Draisci, R., Fagiolo, A., et al. (2003). Determination of enrofloxacin and its metabolite ciprofloxacin in goat milk by high-performance liquid chromatography with diode-array detection: Optimization and validation. Journal of Chromatography A, 987, 221–226.

    Article  CAS  Google Scholar 

  • Council Regulation (1990). 2377/90/EC. Official Journal of the European Community, L224, 1–124.

    Google Scholar 

  • González, C., Moreno, L., Small, J., Jones, D. G., & Sánchez, B. S. F. (2006). A liquid chromatographic method, with fluorometric detection, for the determination of enrofloxacin and ciprofloxacin in plasma and endometrial tissue of mares. Analytica Chimica Acta, 560, 227–234.

    Article  Google Scholar 

  • Hall, Z., Hopley, C., & ÒConnor, G. (2008). High accuracy determination of malachite green and leucomalachite green in salmon tissue by exact matching isotope dilution mass spectrometry. Journal of Chromatography B, 874, 95–100.

    Article  CAS  Google Scholar 

  • Halme, K., Lindfors, E., & Peltonen, K. (2004). Determination of malachite green residues in rainbow trout muscle with liquid chromatography and liquid chromatography coupled with tandem mass spectrometry. Food Additives and Contaminants Part A, 21, 641–648.

    Article  CAS  Google Scholar 

  • Hernandez, M., Aguilar, C., Borrull, F., & Calull, M. (2002). Determination of ciprofloxacin, enrofloxacin and flumequine in pig plasma samples by capillary isotachophoresis–capillary zone electrophoresis. Journal of Chromatography B, 772, 163–172.

    Article  CAS  Google Scholar 

  • Jones, J. J., & Falkinham, J. O. III (2003). Decolorization of malachite green and crystal violet by waterborne pathogenic mycobacteria. Antimicrobial agents and chemotherapy, 47, 2323–2326.

    Article  CAS  Google Scholar 

  • Krebber, R., Hoffend, F. J., & Ruttmann, F. (2009). Simple and rapid determination of enrofloxacin and ciprofloxacin in edible tissues by turbulent flow chromatography/tandem mass spectrometry (TFC–MS/MS). Analytica Chimica Acta, 637, 208–213.

    Article  CAS  Google Scholar 

  • Lee, K. C., Wu, J. L., & Cai, Z. W. (2006). Determination of malachite green and leucomalachite green in edible goldfish muscle by liquid chromatography–ion trap mass spectrometry. Journal of Chromatography B, 843, 247–251.

    Article  CAS  Google Scholar 

  • Li, J. Q. (2009). Study on Stability of Malachite Green by Spectrophotometry. Chinese Journal of Jinzhong University, 26(3), 38–45.

    Google Scholar 

  • Manceau, J., Gicquel, M., Laurentie, M., & Sanders, P. (1999). Simultaneous determination of enrofloxacin and ciprofloxacin in animal biological fluids by high-performance liquid chromatography: Application in pharmacokinetic studies in pig and rabbit. Journal of Chromatography B, 726, 175–184.

    Article  CAS  Google Scholar 

  • Mitrowska, K., Posyniak, A., & Zmudzki, J. (2008). Determination of malachite green and leucomalachite green residues in water using liquid chromatography with visible and fluorescence detection and confirmation by tandem mass spectrometry. Journal of Chromatography A, 1207, 94–100.

    Article  CAS  Google Scholar 

  • Mostafa, S., El-Sadek, M., & Alla, E. A. (2002). Spectrophotometric determination of ciprofloxacin, enrofloxacin and pefloxacin through charge transfer complex formation. Journal of Pharmaceutical and Biomedical Analysis, 27, 133–142.

    Article  CAS  Google Scholar 

  • Muñiz-Valencia, R., Ceballos-Magaña, S. G., Rosales-Martinez, D., Gonzalo-Lumbreras, R., Santos-Montes, A., Cubedo-Fernandez-Trapiella, A., et al. (2008). Method development and validation for melamine and its derivatives in rice concentrates by liquid chromatography. Application to animal feed samples. Analytical Bioanalytical Chemistry, 392, 523–531.

    Article  Google Scholar 

  • Olutosin, R., Idowu, J., & Peggins, O. (2004). Simple, rapid determination of enrofloxacin and ciprofloxacin in bovine milk and plasma by high-performance liquid chromatography with fluorescence detection. Journal of Pharmaceutical and Biomedical Analysis, 35, 143–153.

    Article  Google Scholar 

  • Pedersen, K., & Wedderkopp, A. (2003). Resistance to quinolones in campylobacter jejuni and campylobacter coli from danish broilers at farm level. Journal of Applied Microbiology, 94, 111–119.

    Article  CAS  Google Scholar 

  • Pourreza, N., & Elhami, S. (2007). Spectrophtometric determination of malachite green in fish farming water samples after cloud point extraction using nonionic surfactant Triton X-100. Analytica Chimica Acta, 596, 62–65.

    Article  CAS  Google Scholar 

  • Qin, S. T., Liang, S. T., & Liu, Q. Y. (2009). Characteristic of enrofloxacin ahd its application in prevention and cure of pig disease. Chinese Guangdong Feed, 18(4), 26–27.

    Google Scholar 

  • Ramos, M., Aranda, A., Garcia, E., Reuvers, T., & Hooghuis, H. (2003). Simple and sensitive determination of five quinolones in food by liquid chromatography with fluorescence detection. Journal of Chromatography B, 789, 373–381.

    Article  CAS  Google Scholar 

  • Scherpenisse, P., & Bergwerff, A. A. (2005). Determination of residues of malachite green in finfish by liquid chromatography tandem mass spectrometry. Analytica Chimica Acta, 529, 173–177.

    Article  CAS  Google Scholar 

  • Stammati, A., Nebbia, C., Angelis, I. D., Albo, A. G., Carletti, M., Rebecchi, C., et al. (2005). Effects of malachite green (MG) and its major metabolite, leucomalachite green (LMG), in two human cell lines. Toxicology in Vitro, 19, 853–858.

    Article  CAS  Google Scholar 

  • Srivastava, S., Sinha, R., & Roy, D. (2004). Toxicological effects of malachite green. Aquatic Toxicology, 66, 319–329.

    Article  CAS  Google Scholar 

  • Sun, C., Han, Y. C., Feng, Z., Hu, S. Z., Wu, T., & Tang, S. X. (2001). Stability test for the solution of the dissoluble powder of ciprofloxacin lactate. Agriculture and Technology, 21(6), 92–93.

    Google Scholar 

  • Sunderland, J., Lovering, A. M., Tobin, C. M., MacGowan, A. P., Roe, J. M., & Delsol, A. A. (2004). A reverse-phase HPLC assay for the simultaneous determination of enrofloxacin and ciprofloxacin in pig faeces. International Journal of Antimicrobial Agents, 23, 390–393.

    Article  CAS  Google Scholar 

  • Valle, L., Díaz, C., Zanocco, A. L., & Richter, P. (2005). Determination of the sum of malachite green and leucomalachite green in salmon muscle by liquid chromatography–atmospheric pressure chemical ionisation-mass spectrometry. Journal of Chromatography A, 1067, 101–105.

    Article  CAS  Google Scholar 

  • Wu, X. L., Zhang, G., Wu, Y. N., Hou, X. L., & Yuan, Z. H. (2007). Simultaneous determination of malachite green, gentian violet and their leuco-metabolites in aquatic products by high-performance liquid chromatography–linear ion trap mass spectrometry. Journal of Chromatography A, 1172, 121–126.

    Article  CAS  Google Scholar 

  • Zhang, L. R., Wang, Y. M., Chen, B. Y., & Cheng, N. N. (2003). Neurotoxicity of fluoroquinolones on freely moving rats. Acta Pharmacologica Sinica, 24, 605–609.

    CAS  Google Scholar 

  • Zhou, X. M., Xing, D., Zhu, D. B., Tang, Y. B., & Jia, L. (2008). Development and application of a capillary electrophoresis–electrochemiluminescent method for the analysis of enrofloxacin and its metabolite ciprofloxacin in milk. Talanta, 75, 1300–1306.

    Article  CAS  Google Scholar 

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Correspondence to Hanwen Sun.

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Sun, H., Wang, L., Qin, X. et al. Simultaneous determination of malachite green, enrofloxacin and ciprofloxacin in fish farming water and fish feed by liquid chromatography with solid-phase extraction. Environ Monit Assess 179, 421–429 (2011). https://doi.org/10.1007/s10661-010-1745-4

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  • DOI: https://doi.org/10.1007/s10661-010-1745-4

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