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.
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.
Bergwerff, A. A., & Scherpenisse, P. (2003). Determination of residues of malachite green in aquatic animals. Journal of Chromatography B, 788, 351–359.
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.
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.
Council Regulation (1990). 2377/90/EC. Official Journal of the European Community, L224, 1–124.
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.
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.
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.
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.
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.
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.
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.
Li, J. Q. (2009). Study on Stability of Malachite Green by Spectrophotometry. Chinese Journal of Jinzhong University, 26(3), 38–45.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
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.
Srivastava, S., Sinha, R., & Roy, D. (2004). Toxicological effects of malachite green. Aquatic Toxicology, 66, 319–329.
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.
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.
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.
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.
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.
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.
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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