In‐house validation of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in muscle according to Decision 2002/657/EC

Vinci, Floriana; Guadagnuolo, Grazia; Danese, Vincenzo; Salini, Marco; Serpe, Luigi; Gallo, Pasquale

doi:10.1002/rcm.2200

Cited by 26 publications

(7 citation statements)

References 15 publications

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“…All these transitions were investigated. The most intense ion m/z 152 is the obvious choice as quantitative ion, while m/z 257 and m/z 194 were investigated to find the best confirmatory ion (Vinci et al 2005). Deuterated CAP (d 5 -CAP) was introduced as internal standard and, for the same reasons, the monitored ion was m/z 326!157.…”

Section: Resultsmentioning

confidence: 99%

Validation of a rapid and sensitive routine method for determination of chloramphenicol in honey by LC–MS/MS

Taka

Baras

Bet

2012

Food Additives & Contaminants: Part A

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Chloramphenicol (CAP) is a broad spectrum antibiotic used in the treatment of human and animal diseases. However, CAP can exhibit toxic effects in certain susceptible individuals, causing bone marrow depression, including fatal aplastic anemia. As this condition is dose-independent, CAP has been banned for use in food-producing animals, including honeybees. In this study, a quick, simple and low-cost routine analytical method was developed for the screening and confirmation of chloramphenicol in honey by LC-MS/MS. Sample clean-up takes only two steps without SPE procedure and with recoveries >97%. Honey samples were selected from several producers in Brazil and diluted in a small amount of water. After fortification and addition of d (s)-chloramphenicol as internal standard, the samples were extracted with ethyl acetate. Complete validation of the method was performed on the basis of EU decision 2002/657. Within-laboratory CV reproducibility at the lowest concentration was <10%. An evaluation of two different methods to calculate the decision limit and detection capability gave 0.08 µg kg(-1) for CCα and 0.12 µg kg(-1) for CCβ.

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Section: Resultsmentioning

confidence: 99%

Validation of a rapid and sensitive routine method for determination of chloramphenicol in honey by LC–MS/MS

Taka

Baras

Bet

2012

Food Additives & Contaminants: Part A

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“…The MS/MS spectra of the NSAID standards in the matrix and in the spiked samples were comparable at each contamination level, according to the tolerances set by Decision 2002/657/EC 19, 20…”

Section: Resultsmentioning

confidence: 99%

Determination of fourteen non‐steroidal anti‐inflammatory drugs in animal serum and plasma by liquid chromatography/mass spectrometry

Vinci

Fabbrocino

Fiori

et al. 2006

Rapid Comm Mass Spectrometry

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The European Union has regulated the use of non-steroidal anti-inflammatory drugs (NSAIDs) in animal production and requires its member states to detect their residues in different matrices. In this work, a detailed MS and MS/MS study by ion-trap mass spectrometry of fourteen NSAIDs is described. Two multi-residue reversed-phase LC/ESI-MS/MS methods were developed, one for the determination of salicylic acid, naproxen, carprofen, flurbiprofen, ibuprofen, niflumic acid and meclofenamic acid in the negative ion mode, and the other for the determination of ketoprofen, suxibutazone, diclofenac, mefenamic acid, tolfenamic acid, phenylbutazone and its metabolite oxyphenbutazone in the positive ion mode. It was thus possible to confirm up to 14 different NSAID residues in serum and plasma samples of farmed animals, after chromatographic separation by a linear gradient. These substances were chosen as representative of different chemical subclasses of NSAIDs. The two methods were also validated in-house at three contamination levels, evaluating specificity and calculating mean recoveries, repeatability and within-laboratory reproducibility. The MS/MS product ion spectra were successfully used for the qualitative identification of all the drugs tested. All the NSAIDs, apart from salicylic acid, were recovered in high amounts, ranging between 71.6% and 100.9%.

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“…For animal tissues, fish and shellfish and egg samples, extraction with ethyl acetate (Bogusz et al, 2004), with basic (2 % ammonium hydroxide) ethyl acetate (Zhang et al, 2008) or with acetonitrile (Rønning et al, 2006) is used, together with liquid/liquid partitioning with hexane (Hammack et al, 2003;Vinci et al, 2005;Yibar et al, 2011;Douny et al, 2013) or with petroleum ether and isooctane (Tyagi et al, 2008) to remove fat. Further clean-up of the extract is carried out using SPE on silica , on a reversed phase polymeric sorbent (Gikas et al, 2004), on C 18 (Gantverg et al, 2003), on a cation exchange sorbent (Xia et al, 2013) or on graphene (Wu et al, 2012).…”

Section: Confirmatory Methodsmentioning

confidence: 99%

Scientific Opinion on Chloramphenicol in food and feed

2014

EFS2

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Chloramphenicol is an antibiotic not authorised for use in food-producing animals in the European Union (EU). However, being produced by soil bacteria, it may occur in plants. The European Commission asked EFSA for a scientific opinion on the risks to human and animal health related to the presence of chloramphenicol in food and feed and whether a reference point for action (RPA) of 0.3 µg/kg is adequate to protect public and animal health. Data on occurrence of chloramphenicol in food extracted from the national residue monitoring plan results and from the Rapid Alert System for Food and Feed (RASFF) were too limited to carry out a reliable human dietary exposure assessment. Instead, human dietary exposure was calculated for a scenario in which chloramphenicol is present at 0.3 µg/kg in all foods of animal origin, foods containing enzyme preparations and foods which may be contaminated naturally. The mean chronic dietary exposure for this worst-case scenario would range from 11 to 17 and 2.2 to 4.0 ng/kg b.w. per day for toddlers and adults, respectively. The potential dietary exposure of livestock to chloramphenicol was estimated to be below 1 µg/kg b.w. per day. Chloramphenicol is implicated in the generation of aplastic anaemia in humans and causes reproductive/hepatotoxic effects in animals. Margins of exposure for these effects were calculated at 2.4 × 10 5 or greater and the CONTAM Panel concluded that it is unlikely that exposure to food contaminated with chloramphenicol at or below 0.3 µg/kg is a health concern for aplastic anaemia or reproductive/hepatotoxic effects. Chloramphenicol exhibits genotoxicity but, owing to the lack of data, the risk of carcinogenicity cannot be assessed. The SUMMARYChloramphenicol is a broad-spectrum antibiotic effective against Gram-positive and Gram-negative bacteria and, in the past, has been widely used to treat infections in both humans and animals. Chloramphenicol is not authorised for use in food-producing animals in the European Union (EU) but may be used in human medicine and in treatments for non-food-producing animals. Apart from its potential occurrence as a residue in food from illicit treatment of food-producing animals, chloramphenicol has also been used in feed and food enzyme products and may occur naturally in plants from its production by the soil bacterium Streptomyces venezuelae.The EFSA Scientific Opinion entitled "Guidance on methodological principles and scientific methods to be taken into account when establishing Reference Points for Action (RPAs) for non-allowed pharmacologically active substances present in food of animal origin" identified an approach for establishing RPAs for various categories of non-allowed pharmacologically active substances. However, the opinion also identified certain categories of non-allowed pharmacologically active substances that are considered to be outside the scope of the procedure, including substances causing blood dyscrasias (aplastic anaemia) such as chloramphenicol. As chloramphenicol is excluded fro...

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In‐house validation of a liquid chromatography/electrospray tandem mass spectrometry method for confirmation of chloramphenicol residues in muscle according to Decision 2002/657/EC

Cited by 26 publications

References 15 publications

Validation of a rapid and sensitive routine method for determination of chloramphenicol in honey by LC–MS/MS

Validation of a rapid and sensitive routine method for determination of chloramphenicol in honey by LC–MS/MS

Determination of fourteen non‐steroidal anti‐inflammatory drugs in animal serum and plasma by liquid chromatography/mass spectrometry

Scientific Opinion on Chloramphenicol in food and feed

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