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A high-throughput UHPLC method for the analysis of 5-nitroimidazole residues in milk based on salting-out assisted liquid-liquid extraction.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 15; 1068-1069:125-130.JC

Abstract

A novel salting-out assisted liquid-liquid extraction (SALLE) method has been developed for the extraction of eight 5-NDZ antibiotics from milk samples prior to their analysis by UHPLC. An exhaustive study of the parameters involved in the SALLE procedure has been carried out, optimizing the extraction solvent volume, the amount of the salt agent, and the centrifugation and vortex timing by an experimental design. After sample treatment, the obtained extract was reconstituted in the mobile phase (6:94 (v/v) acetonitrile/water containing 0.1% (v/v) of formic acid) and analyzed by the proposed UHPLC-UV method. Separation was accomplished in a C18 Zorbax Eclipse Plus (50mm×2.1mm, 1.8μm) column at 45°C within 8min. Gradient mode was considered using a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and acetonitrile containing 0.1% (v/v) formic acid at a flow rate of 0.45mL/min. Analytical signals were monitored at 320nm. Matrix-matched calibration curves showed satisfactory linearity (R2≥0.996). LODs, ranging from 2 to 4μg/L, were achieved and precision studies showed RSDs lower than 12.8% in terms of peak height. Additionally, recoveries higher than 62.8% were obtained for all studied compounds in milk samples.

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Publisher Full Text (DOI)

Authors+Show Affiliations

Hernández-Mesa M
Department of Analytical Chemistry, Faculty of Sciences, University of Granada,Av. Fuentenueva s/n, E-18071 Granada, Spain.
Carbonell-Rozas L
Department of Analytical Chemistry, Faculty of Sciences, University of Granada,Av. Fuentenueva s/n, E-18071 Granada, Spain.
Cruces-Blanco C
Department of Analytical Chemistry, Faculty of Sciences, University of Granada,Av. Fuentenueva s/n, E-18071 Granada, Spain.
García-Campaña AM
Department of Analytical Chemistry, Faculty of Sciences, University of Granada,Av. Fuentenueva s/n, E-18071 Granada, Spain. Electronic address: amgarcia@ugr.es.

MeSH

AnimalsCattleChromatography, High Pressure LiquidDrug ResiduesHigh-Throughput Screening AssaysLimit of DetectionLinear ModelsLiquid-Liquid ExtractionMilkNitroimidazolesReproducibility of ResultsSodium Chloride

Pub Type(s)

Journal Article

Language

eng

PubMed ID

29059587

Citation

Hernández-Mesa, Maykel, et al. "A High-throughput UHPLC Method for the Analysis of 5-nitroimidazole Residues in Milk Based On Salting-out Assisted Liquid-liquid Extraction." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 1068-1069, 2017, pp. 125-130.
Hernández-Mesa M, Carbonell-Rozas L, Cruces-Blanco C, et al. A high-throughput UHPLC method for the analysis of 5-nitroimidazole residues in milk based on salting-out assisted liquid-liquid extraction. J Chromatogr B Analyt Technol Biomed Life Sci. 2017;1068-1069:125-130.
Hernández-Mesa, M., Carbonell-Rozas, L., Cruces-Blanco, C., & García-Campaña, A. M. (2017). A high-throughput UHPLC method for the analysis of 5-nitroimidazole residues in milk based on salting-out assisted liquid-liquid extraction. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 1068-1069, 125-130. https://doi.org/10.1016/j.jchromb.2017.10.016
Hernández-Mesa M, et al. A High-throughput UHPLC Method for the Analysis of 5-nitroimidazole Residues in Milk Based On Salting-out Assisted Liquid-liquid Extraction. J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 15;1068-1069:125-130. PubMed PMID: 29059587.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - A high-throughput UHPLC method for the analysis of 5-nitroimidazole residues in milk based on salting-out assisted liquid-liquid extraction. AU - Hernández-Mesa,Maykel, AU - Carbonell-Rozas,Laura, AU - Cruces-Blanco,Carmen, AU - García-Campaña,Ana M, Y1 - 2017/10/13/ PY - 2017/06/30/received PY - 2017/09/25/revised PY - 2017/10/07/accepted PY - 2017/10/24/pubmed PY - 2017/12/5/medline PY - 2017/10/24/entrez KW - 5-Nitroimidazoles KW - Milk KW - Salting out-assisted liquid–liquid extraction KW - Ultra-high performance liquid chromatography SP - 125 EP - 130 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 1068-1069 N2 - A novel salting-out assisted liquid-liquid extraction (SALLE) method has been developed for the extraction of eight 5-NDZ antibiotics from milk samples prior to their analysis by UHPLC. An exhaustive study of the parameters involved in the SALLE procedure has been carried out, optimizing the extraction solvent volume, the amount of the salt agent, and the centrifugation and vortex timing by an experimental design. After sample treatment, the obtained extract was reconstituted in the mobile phase (6:94 (v/v) acetonitrile/water containing 0.1% (v/v) of formic acid) and analyzed by the proposed UHPLC-UV method. Separation was accomplished in a C18 Zorbax Eclipse Plus (50mm×2.1mm, 1.8μm) column at 45°C within 8min. Gradient mode was considered using a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and acetonitrile containing 0.1% (v/v) formic acid at a flow rate of 0.45mL/min. Analytical signals were monitored at 320nm. Matrix-matched calibration curves showed satisfactory linearity (R2≥0.996). LODs, ranging from 2 to 4μg/L, were achieved and precision studies showed RSDs lower than 12.8% in terms of peak height. Additionally, recoveries higher than 62.8% were obtained for all studied compounds in milk samples. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/29059587/A_high_throughput_UHPLC_method_for_the_analysis_of_5_nitroimidazole_residues_in_milk_based_on_salting_out_assisted_liquid_liquid_extraction_ DB - PRIME DP - Unbound Medicine ER -

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