Single-laboratory validation of an LC-MS/MS method for determining florfenicol (FF) and florfenicol amine (FFA) residues in chicken feathers and application to a residue-depletion study

Cornejo, Javiera; Pokrant, Ekaterina; Riquelme, Ricardo; Briceño, Cristóbal; Maddaleno, Aldo; Araya-Jordán, C.; Martín, Betty San

doi:10.1080/19440049.2016.1267876

Cited by 21 publications

(13 citation statements)

References 20 publications

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“…The results in this study agree with previous works and are particularly similar to those observed by Cornejo et al [ 30 ], as the concentrations of FF and FFA persisted for a longer period of time in chicken claws than the withdrawal time currently established in muscle tissues for the commercial formulation. Furthermore, for each sampling point, residue concentrations of these analytes were detectable at greater concentrations in claws than in samples of muscle and liver tissues that were sourced from the same animals.…”

Section: Discussionsupporting

confidence: 93%

Residue Depletion of Florfenicol and Florfenicol Amine in Broiler Chicken Claws and a Comparison of Their Concentrations in Edible Tissues Using LC–MS/MS

et al. 2018

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Antimicrobial residues might persist in products and by-products destined for human or animal consumption. Studies exploring the depletion behavior of florfenicol residues in broiler chicken claws are scarce, even though claws can enter the food chain directly or indirectly. Hence, this study intended to assess the concentrations of florfenicol (FF) and florfenicol amine (FFA)—its active metabolite—in chicken claws from birds that were treated with a therapeutic dose of florfenicol. Furthermore, concentrations of these analytes in this matrix were compared with their concentrations in edible tissues at each sampling point. A group of 70 broiler chickens were raised under controlled conditions and used to assess residue depletion. Sampling points were on days 5, 10, 20, 25, 30, 35, and 40 after ceasing treatment, thus extending beyond the withdrawal period established for muscle tissue (30 days). Analytes were extracted using HPLC-grade water and acetone, and dichloromethane was used for the clean-up stage. Liquid chromatography coupled to mass spectroscopy detection (LC–MS/MS) was used to detect and quantify the analytes. The analytical methodology developed in this study was validated in-house and based on the recommendations described in the Commission Decision 2002/657/EC from the European Union. Analyte concentrations were calculated by linear regression analysis of calibration curves that were fortified using an internal standard of chloramphenicol-d5 (CAF-d5). The depletion time of FF and FFA was set at 74 days in claws, based on a 95% confidence level and using the limit of detection (LOD) as the cut-off point. Our findings show that FF and FFA can be found in chicken claws at higher concentrations than in muscle and liver samples at each sampling point.

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Section: Discussionsupporting

confidence: 93%

Residue Depletion of Florfenicol and Florfenicol Amine in Broiler Chicken Claws and a Comparison of Their Concentrations in Edible Tissues Using LC–MS/MS

et al. 2018

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“…In another study by Cornejo et al [ 25 ], they determined that residues of florfenicol and florfenicol amine also remained in feathers for longer periods than the withdrawal time that has been established for muscle tissue.…”

Section: Discussionmentioning

confidence: 99%

“…In the case of muscle and liver samples, the first step to process them was the removal of fats and grinding. Meanwhile, feather samples were first treated cryogenically with liquid nitrogen, as different studies have reported that this procedure improves grinding efficiency of feathers [ 23 , 25 , 26 ]. Then, samples were ground in an industrial Robot Coupe ® R4 table-top cutter food processor (Burgundy, France) to ensure their homogeneity.…”

Section: Methodsmentioning

confidence: 99%

Determination of sulfachloropyridazine residue levels in feathers from broiler chickens after oral administration using liquid chromatography coupled to tandem mass spectrometry

et al. 2018

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Several antimicrobials are routinely used by the poultry farming industry on their daily operations, however, researchers have found for some antimicrobials that their residues persist for longer periods in feathers than they do in edible tissues, and at higher concentrations, as well. But this information is not known for other classes of antimicrobials, such as the sulfonamides. Therefore, this work presents an accurate and reliable analytical method for the detection of sulfachloropyridazine (SCP) in feathers and edible tissues from broiler chickens. This method was also validated in-house and then used to study the depletion of sulfachloropyridazine in those matrices. The experimental group comprised 54 broiler chickens, who were raised under controlled conditions and then treated with a commercial formulation of 10% sulfachloropyridazine for 5 days. Samples were analyzed via LC-MS/MS, using 13C6-sulfamethazine (SMZ-13C6) as an internal standard. Aromatic sulfonic acid solid phase extraction (SPE) cartridges were used to clean up the samples. The Limit of Detection (LOD) for this method was set at 10 μg kg-1 on feathers and liver; and at 5 μg kg-1 on muscle. Within the range of 10–100 μg kg-1, the calibration curves for all matrices presented a determination coefficient greater than 0.96. Our results show, with a 95% confidence level, that sulfachloropyridazine persisted in feathers for up to 55 days after ceasing treatment, and its concentrations were higher than in edible tissues. In consequence, to avoid re-entry of antimicrobial residues into the food-chain, we recommend monitoring and inspecting animal diets that contain feather derivatives, such as feathers meals, because they could be sourced from birds that might have been medicated with sulfachloropyridazine.

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“…There is a need for methods that are able to detect the use of antibiotics administered over the entire life span of an animal, including treatments administered during the first days of the animals’ lives. In previous research focusing on the excretion of oxytetracycline [ 7 ], multiple fluoroquinolones (enrofloxacin, its metabolite ciprofloxacin [ 8 ], and flumequin [ 9 ]) and florfenicol and its metabolite florfenicol amine [ 10 ] to feathers, it has already been shown that antibiotic residues can still be detected in feathers long after treatment. In another study, different antibiotics in feather meal, originating from different countries, were detected, including antibiotics that are registered as banned substances in the country of origin [ 11 ].…”

Section: Introductionmentioning

confidence: 99%

The analysis of tetracyclines, quinolones, macrolides, lincosamides, pleuromutilins, and sulfonamides in chicken feathers using UHPLC-MS/MS in order to monitor antibiotic use in the poultry sector

et al. 2017

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In The Netherlands, all antibiotic treatments should be registered at the farm and in a central database. To enforce correct antibiotic use and registration, and to enforce prudent use of antibiotics, there is a need for methods that are able to detect antibiotic treatments. Ideally, such a method is able to detect antibiotic applications during the entire lifespan of an animal, including treatments administered during the first days of the animals’ lives. Monitoring tissue, as is common practice, only provides a limited window of opportunity, as residue levels in tissue soon drop below measurable quantities. The analysis of feathers proves to be a promising tool in this respect. Furthermore, a qualitative confirmatory method was developed for the analyses of six major groups of antibiotics in ground chicken feathers, aiming for a detection limit as low as reasonably possible. The method was validated according to Commission Decision 2002/657/EC. All compounds comply with the criteria and, as a matter of fact, 58% of the compounds could also be quantified according to regulations. Additionally, we demonstrated that a less laborious method, in which whole feathers were analyzed, proved successful in the detection of applied antibiotics. Most compounds could be detected at levels of 2 μg kg−1 or below with the exception of sulfachloropyridazine, tylosin, and tylvalosin. This demonstrates the effectiveness of feather analysis to detect antibiotic use to allow effective enforcement of antibiotic use and prevent the illegal, off-label, and nonregistered use of antibiotics.

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Single-laboratory validation of an LC-MS/MS method for determining florfenicol (FF) and florfenicol amine (FFA) residues in chicken feathers and application to a residue-depletion study

Cited by 21 publications

References 20 publications

Residue Depletion of Florfenicol and Florfenicol Amine in Broiler Chicken Claws and a Comparison of Their Concentrations in Edible Tissues Using LC–MS/MS

Residue Depletion of Florfenicol and Florfenicol Amine in Broiler Chicken Claws and a Comparison of Their Concentrations in Edible Tissues Using LC–MS/MS

Determination of sulfachloropyridazine residue levels in feathers from broiler chickens after oral administration using liquid chromatography coupled to tandem mass spectrometry

The analysis of tetracyclines, quinolones, macrolides, lincosamides, pleuromutilins, and sulfonamides in chicken feathers using UHPLC-MS/MS in order to monitor antibiotic use in the poultry sector

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