Multilaboratory Validation of a Method To Confirm Chloramphenicol in Shrimp and Crabmeat by Liquid Chromatography-Tandem Mass Spectrometry

Hammack, Walter; Carson, Mary C; Neuhaus, Barbara; Hurlbut, Jeffrey A.; Nochetto, Cristina; Stuart, James S; Brown, Amy N; Kilpatrick, Donna; Youngs, Kristl; Ferbos, Krystle; Heller, David

doi:10.1093/jaoac/86.6.1135

Cited by 20 publications

(6 citation statements)

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“…LC/MS has been used to detect CAP and sulfonamides in a variety of food matrices and provides improved selectivity over fluorescence or UV detection – . More recently, LC/tandem mass spectrometry (MS/MS) detection methods have been successful in determining CAP and sulfonamides in the low ng/g (ppb) level in a variety of matrices including honey – . Nowadays, tandem mass spectrometry is the preferred technique, as it provides improved selectivity and sensitivity over other techniques.…”

Section: Introductionmentioning

confidence: 99%

Analysis and Occurrence of 14 Sulfonamide Antibacterials and Chloramphenicol in Honey by Solid-Phase Extraction Followed by LC/MS/MS Analysis

Sheridan

Policastro

Thomas

et al. 2008

J. Agric. Food Chem.

116

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A method was developed for the analysis of 14 sulfonamide antibiotics and chloramphenicol in honey. These antibiotics have been banned for use in food-producing animals; yet, their residues were found in many samples, illustrating the need for a multiresidue analysis for these antibiotics in honey. The method described here uses an acid hydrolysis step to liberate the sugar-bound sulfonamides followed by a solid-phase extraction to remove potential interferences. Analysis was by liquid chromatography--electrospray ionization--tandem mass spectrometry in negative mode for all 15 analytes. This MRM method generated two structurally significant transitions per compound, and it was designed to conform to U.S. Food and Drug Administration MS confirmation guidelines. It also provides 4-EU identification points. One hundred sixteen samples from 25 countries were analyzed, and 38% were found to contain at least one target antimicrobial. Five different target compounds were found in honey from 13 different countries.

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Section: Introductionmentioning

confidence: 99%

Analysis and Occurrence of 14 Sulfonamide Antibacterials and Chloramphenicol in Honey by Solid-Phase Extraction Followed by LC/MS/MS Analysis

Sheridan

Policastro

Thomas

et al. 2008

J. Agric. Food Chem.

116

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“…Typically, the method performance level required for CAP has been below 1 ng/g. This Q-TOF multiclass screening method is not as sensitive as dedicated (single residue) triple-quadrupole LC-MS/MS methods. , However, even though the 1 X level for CAP was set to 1 ng/g in this method, CAP was detected in samples ( n = 6) fortified at half that level (0.5 ng/g).…”

Section: Resultsmentioning

confidence: 99%

Analysis of Veterinary Drug Residues in Frog Legs and Other Aquacultured Species Using Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Turnipseed

Clark

Storey

et al. 2012

J. Agric. Food Chem.

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A liquid chromatography quadrupole time-of-flight (Q-TOF) mass spectrometry method was developed to analyze veterinary drug residues in frog legs and other aquacultured species. Samples were extracted using a procedure based on a method developed for the analysis of fluoroquinolones (FQs) in fish. Briefly, the tissue was extracted with dilute acetic acid and acetonitrile with added sodium chloride. After centrifugation, the extracts were evaporated and reconstituted in mobile phase. A molecular weight cutoff filter was used to clean up the final extract. A set of target compounds, including trimethoprim, sulfamethoxazole, chloramphenicol, quinolones, and FQs, was used to validate the method. Screening of residues was accomplished by collecting TOF (MS¹) data and comparing the accurate mass and retention times of compounds to a database containing information for veterinary drugs. An evaluation of the MS data in fortified frog legs indicated that the target compounds could be consistently detected at the level of concern. The linearity and recoveries from matrix were evaluated for these analytes to estimate the amount of residue present. MS/MS data were also generated from precursor ions, and the mass accuracy of the product ions for each compound was compared to theoretical values. When the method was used to analyze imported frog legs, many of these residues were found in the samples, often in combination and at relatively high concentrations (>10 ng/g). The data from these samples were also evaluated for nontarget analytes such as residue metabolites and other chemotherapeutics.

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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 (Mottier et al, 2003), 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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Multilaboratory Validation of a Method To Confirm Chloramphenicol in Shrimp and Crabmeat by Liquid Chromatography-Tandem Mass Spectrometry

Cited by 20 publications

References 1 publication

Analysis and Occurrence of 14 Sulfonamide Antibacterials and Chloramphenicol in Honey by Solid-Phase Extraction Followed by LC/MS/MS Analysis

Analysis and Occurrence of 14 Sulfonamide Antibacterials and Chloramphenicol in Honey by Solid-Phase Extraction Followed by LC/MS/MS Analysis

Analysis of Veterinary Drug Residues in Frog Legs and Other Aquacultured Species Using Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

Scientific Opinion on Chloramphenicol in food and feed

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