Multiclass method for the determination of quinolones and β-lactams, in raw cow milk using dispersive liquid–liquid microextraction and ultra high performance liquid chromatography–tandem mass spectrometry

Junza, Alexandra; Dorival-García, Noemí; Zafra-Gómez, A.; Barrón, D.; Ballesteros, O.; Barbosa, J.; Navalón, Alberto

doi:10.1016/j.chroma.2014.06.034

Cited by 80 publications

(43 citation statements)

References 39 publications

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“…However, it is well known that reverse‐phase SPE led to unsatisfactory recoveries for the more hydrophilic and hydrophobic compounds due to its inherent selectivity . Finally, four papers described a generic procedure not attributable to any of the three over mentioned strategies (‘others’) . In these procedures, generally after deproteinization step, no further purification was carried out.…”

Section: Introductionmentioning

confidence: 99%

Multiclass method for the determination of 62 antibiotics in milk

et al. 2016

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A multiclass method for screening and confirmatory analysis of antimicrobial residues in milk has been developed and validated. Sixty-two antibiotics belonging to ten different drug families (amphenicols, cephalosporins, lincosamides, macrolides, penicillin, pleuromutilins, quinolones, rifamycins, sulfonamides and tetracyclines) have been included. After the addition of an aqueous solution of EDTA, the milk samples were extracted twice with acetonitrile, evaporated and dissolved in ammonium acetate. After centrifugation, 10 µl were analysed using LC-Q-Orbitrap operating in positive electrospray ionization mode. The method was validated in bovine milk in the range 2-150 µg kg(-1) for all antibiotics; for four compounds with maximum residue limits higher than 100 µg kg(-1) , the validation interval has been extended until 333 µg kg(-1) . The estimated performance characteristics were satisfactory complying with the requirements of Commission Decision 2002/657/EC. Good accuracies were obtained also taking advantage from the versatility of the hybrid mass analyser. Identification criteria were achieved verifying the mass accuracy and ion ratio of two ions, including the pseudomolecular one, where possible. Finally, the developed procedure was applied to 13 real cases of suspect milk samples (microbiological assay) confirming the presence of one or more antibiotics, although frequently, the maximum residue limits were not exceeded. The availability of rapid multiclass confirmatory methods can avoid wastes of suspect, but compliant, raw milk samples. Copyright © 2016 John Wiley& Sons, Ltd.

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Section: Introductionmentioning

confidence: 99%

Multiclass method for the determination of 62 antibiotics in milk

et al. 2016

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“…Finally, a comparison with other published methods was conducted with the aim to show the advantages of the method reported in this paper. In the literature, the number of FQs that can be determined simultaneously in a less complex matrix than porcine blood is less than eight . Consequently, it is apparent that one important achievement is the possibility to quantitate the nine analytes together.…”

Section: Resultsmentioning

confidence: 99%

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Validation of a CE method using univariate calibration or multivariate curve resolution‐alternating least squares for overlapped peaks

2017

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In the previously published part of this study, we detailed a novel strategy based on dispersive liquid-liquid microextraction to extract and preconcentrate nine fluoroquinolones in porcine blood. Moreover, we presented the optimized experimental conditions to obtain complete CE separation between target analytes. Consequently, this second part reports the validation of the developed method to determine flumenique, difloxacin, enrofloxacin, marbofloxacin, ofloxacin, ciprofloxacin, through univariate calibration, and enoxacin, danofloxacin, and gatifloxacin through multivariate curve resolution analysis. The validation was performed according to FDA guidelines for bioanalytical assay procedures and the European Directive 2002/657 to demonstrate that the results are reliable. The method was applied for the determination of fluoroquinolones in real samples. Results indicated a high selectivity and excellent precision characteristics, with RSD less than 11.9% in the concentrations, in intra- and interassay precision studies. Linearity was proved for a range from 4.00 to 30.00 mg/L and the recovery has been investigated at four different fortification levels, from 89 to 113%. Several approaches found in the literature were used to determinate the LODs and LOQs. Though all strategies used were appropriate, we obtained different values when using different methods. Estimating the S/N ratio with the mean noise level in the migration time of each fluoroquinolones turned out as the best studied method for evaluating the LODs and LOQs, and the values were in a range of 1.55 to 4.55 mg/L and 5.17 to 9.62 mg/L, respectively.

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“…DAN constitutes one of the most used antibiotics and its determination involves multiple steps of sample preparation followed by expensive chromatographic techniques, 22,23 sometimes coupled with mass spectrometry. DAN constitutes one of the most used antibiotics and its determination involves multiple steps of sample preparation followed by expensive chromatographic techniques, 22,23 sometimes coupled with mass spectrometry.…”

Section: Introductionmentioning

confidence: 99%

β-Cyclodextrin decorated nanocellulose: a smart approach towards the selective fluorimetric determination of danofloxacin in milk samples

Ruiz-Palomero

Soriano

Valcárcel

2015

Analyst

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An innovative and versatile strategy of Solid Phase Microextraction (SPME) is shown by using a new type of β-cyclodextrin-modified nanocellulose (CD-NC) as a sorbent material. β-cyclodextrin (used as an inclusion-type selector) was covalently bonded to amine-modified nanocellulose by an amidation reaction. Such novel nanocavities were successfully applied to the selective recognition of danofloxacin (DAN), an antibiotic used to treat animal diseases, via supramolecular host-guest interactions. The SPME methodology, using a platform based on β-cyclodextrin-"decorated" nanocellulose as a sorbent material, showed a wide linear fluorimetric response against DAN from 8 to 800 μg L(-1) and a detection limit of 2.5 μg L(-1). The specific recognition of DAN has been proven to be highly selective and efficient against this metabolite and other fluoroquinolones. The reusability and the high efficiency in the extraction and preconcentration of DAN in milk samples allow recoveries of 94%.

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Multiclass method for the determination of quinolones and β-lactams, in raw cow milk using dispersive liquid–liquid microextraction and ultra high performance liquid chromatography–tandem mass spectrometry

Cited by 80 publications

References 39 publications

Multiclass method for the determination of 62 antibiotics in milk

Multiclass method for the determination of 62 antibiotics in milk

Dispersive liquid–liquid microextraction of quinolones in porcine blood: Validation of a CE method using univariate calibration or multivariate curve resolution‐alternating least squares for overlapped peaks

β-Cyclodextrin decorated nanocellulose: a smart approach towards the selective fluorimetric determination of danofloxacin in milk samples

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