Simultaneous determination of eleven quinolones in animal feed by liquid chromatography with fluorescence and ultraviolet absorbance detection

Galarini, Roberta; Fioroni, Laura; Angelucci, Federico; Tovo, Gloria Raquel; Cristofani, Elisa

doi:10.1016/j.chroma.2009.06.076

Cited by 49 publications

(31 citation statements)

References 22 publications

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“…As a result these should not be found in animal feeds. While there are single class methods for the analysis of some of compounds [Vincent et al, 2008;Galarini et al, 2009;Pecorelli et al, 2003;Barbosa et al, 2007;van Holthoon et al, 2010] [Dusi et al, 2000], amprolium/ethopabate [Tan et al, 1996] and carbadox [Kesiunaite et al, 2008;Hutchinson et al, 2005] while for compounds such as dinitolimide no a Dublin Institute of Technology,School of Chemical and Pharmaceutical Sciences,Kevin Street,Dublin 8,Ireland b State Laboratory,Young's Cross,Backweston Campus,Backweston,Celbridge,Co. Kildare,Ireland.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a rapid multi-class method for the confirmation of fourteen prohibited medicinal additives in pig and poultry compound feed by liquid chromatography–tandem mass spectrometry

Cronly

Behan²,

Foley³

et al. 2010

Journal of Pharmaceutical and Biomedical Analysis

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A confirmatory method has been developed to allow for the analysis of fourteen prohibited medicinal additives in pig and poultry compound feed. These compounds are prohibited for use as feed additives although some are still authorised for use in medicated feed. Feed samples are extracted by acetonitrile with addition of sodium sulphate. The extracts undergo a hexane wash to aid with sample purification. The extracts are then evaporated to dryness and reconstituted in initial mobile phase. The samples undergo an ultracentrifugation step prior to injection onto the LC-MS/MS system and are analysed in a run time of 26 minutes. The LC-MS/MS system is run in MRM mode with both positive and negative electrospray ionisation. The method was validated over three days and is capable of quantitatively analysing for metronidazole, dimetridazole, ronidazole, ipronidazole, chloramphenicol, sulfadiazine, sulfamethazine, dinitolimide, ethopabate, carbadox and clopidol. The method is also capable of qualitatively analysing for tylosin, virginiamycin and avilamycin. A level of 100 µg kg -1 was used for validation purposes and the method is capable of analysing to this level for all the compounds. Validation criteria of trueness, precision, repeatability and reproducibility along with measurement uncertainty are calculated for all analytes.

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Section: Introductionmentioning

confidence: 99%

Development and validation of a rapid multi-class method for the confirmation of fourteen prohibited medicinal additives in pig and poultry compound feed by liquid chromatography–tandem mass spectrometry

Cronly

Behan²,

Foley³

et al. 2010

Journal of Pharmaceutical and Biomedical Analysis

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“…However, the relative percentage standard uncertainty values obtained in this study, which are shown in Table 6; appear to be satisfactory when compared with the reported uncertainties for these compounds in several other matrices. 1,27,28 Evaluation of the limits of detection (LoD) and quantification (LoQ) The limit of detection is defined as the minimum amount of substance that can be detected at a given confidence limit (usually 95%) but not necessarily accurately quantified. It is generally reported as a concentration or amount of substance and it is derived from the smallest signal that can be detected with a reasonable certainty for a particular analytical method.…”

Section: (10)mentioning

confidence: 99%

“…Quinolones were eluted with 3 ml of a mixture methanol-ammonia (75%-25%). 11,28 Samples were evaporated under nitrogen stream at 35ºC reaching almost dryness, the residue was dissolved in 600 μL aqueous formic acid (0.4% v/v) and filtered through a 0,22 µm PVDF membrane. The internal stardard was added and the samples were diluted to 1±0,01 g with aqueous formic acid (0,4% v/v) before injecting 100 µL into the LC-Fl system.…”

Section: Extraction and Clean-upmentioning

confidence: 99%

Validation of a Liquid Chromatography-Fluorescence Spectrometric Method for the Quantification of Four Quinolones in Pig and Chicken Muscle Following the European Union Guideline Ec/657/2002

VASQUEZ-MARTINEZ¹,

R²,

Villa³

et al. 2011

J. Chil. Chem. Soc.

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Quinolones are a group of structurally related antibacterial compounds. Over the last years their use in animal production has been greatly increased. This increase can cause the resistance of bacteria. In order to protect human health the European Union (EU), as well as other countries, has established Maximum Residue Limits (MRL) for these antibacterial agents in several foods. Among these foods, pig and chicken muscle have different MRLs in the sub-ppm range.A liquid chromatography-fluorescence spectrometric method has been developed and validated for the simultaneous assessment of four of the most used quinolones in edible animal matrices production. Simultaneous quantification of enrofloxacin, ciprofloxacin, oxolinic acid and flumequine was achieved by a method involving an initial aqueous extraction step followed by a solid-liquid-phase extraction using reverse-phase columns (C-18) and a final injection of all quinolones in a single chromatographic run using HPLC-Fluorescence detection. Nalidixic acid was used as internal standard.In addition to the description of the analytical method developed for the quantification of the studied quinolones, the different validation parameters of this method according to Commission Decision EC /657/2002 of the EU are presented and discussed.

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“…Thorough reviews on the recent advances in quinolones determination in food and environmental samples have been published [1,2,5,7]. The mostly reported methods are based on liquid chromatography coupled with fluorescence detection (FD) [4,5,[8][9][10][11][12] or different mass spectrometric techniques (MS) [3,[13][14][15][16][17][18]. Almost all of them are multiresidue methods aiming to increase the rapidity and simplicity of the existing ones.…”

Section: Introductionmentioning

confidence: 99%

Determination of quinolonones in food of animal origin by liquid chromatography coupled with fluorescence and mass spectrometric detection

Stoilova¹,

Surleva²,

Stoev³

2014

Acta Chromatographica

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Summary. High-performance liquid chromatography coupled with fluorescence (HPLC-FD) and tandem mass spectrometric detection (LC-MS/MS) was studied as a versatile tool for fast and reliable determination of nine regulated quinolones in food of animal origin (Council Regulation 2377/90/ECC). The sample pre-treatment protocol includes double step extraction with acetonitrile followed by solid phase extraction (SPE) cleanup on hydrophobic-lipophilic balance (HLB) cartridge. The separation of quinolones in HPLC-FD determination was performed on C18 Zorbax column with a gradient mixture of aqueous formic acid, methanol, and acetonitrile. A multi-wavelength excitation/emission program was used for sensitive quinolones detection. The separation efficiency of newly available chromatographic columns: Gemini C18 and Synergi Polar RP (fully porous particles), as well as Kinetex PFP and Poroshell 120 EC-C18 (coreshell particles), was studied in liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) analysis. Appropriate gradient elution program was designed for each column. Multiple reaction monitoring was used for selective determination of each quinolone. LC-MS/MS allowed quinolones determination in less than 5 min. Both methods showed detection limits below maximum residue limits for quinolones residues in food commodities.

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Simultaneous determination of eleven quinolones in animal feed by liquid chromatography with fluorescence and ultraviolet absorbance detection

Cited by 49 publications

References 22 publications

Development and validation of a rapid multi-class method for the confirmation of fourteen prohibited medicinal additives in pig and poultry compound feed by liquid chromatography–tandem mass spectrometry

Development and validation of a rapid multi-class method for the confirmation of fourteen prohibited medicinal additives in pig and poultry compound feed by liquid chromatography–tandem mass spectrometry

Validation of a Liquid Chromatography-Fluorescence Spectrometric Method for the Quantification of Four Quinolones in Pig and Chicken Muscle Following the European Union Guideline Ec/657/2002

Determination of quinolonones in food of animal origin by liquid chromatography coupled with fluorescence and mass spectrometric detection

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