Abstract
A rapid and reliable method using liquid chromatography (UHPLC) tandem mass spectrometry (MS/MS) to identify and quantify chloramphenicol (CAP), thiamphenicol (TAP), florfenicol (FF) and its marker residue florfenicol amine (FFA) has been developed and validated. FF and TAP are both allowed substances and different MRLs have been established for different matrices and species. However, CAP is a well-known forbidden substance with a MRPL of 0.3 μg kg−1 for all matrices. It was relevant to develop this confirmatory method to quantify simultaneously the four amphenicols in kidney and muscle of all species, to make more effective the official control programme for this group of substances. The variety of levels of interest to be studied for the allowed compounds and the different chemical behaviour of FFA have been the main difficulties in the development and validation of the method. The method has been validated in swine, bovine, caprine, equine, porcine, aquaculture species, rabbit and poultry muscle and kidney (except aquaculture species, rabbit and poultry). Performance criteria have been calculated in accordance with Commission Decision 2002/657/EC. The proposed procedure is being applied to the official control in the Valencian Region after being successfully evaluated by ENAC (Spanish national body for the accreditation).
Similar content being viewed by others
References
Commission Decision (2002) Commission decision 2002/657/EC of 12 august 2002 concerning the performance of analytical methods and the interpretation of results. Off J Eur Communities L 221:8
Commission Decision (2003) Commission decision 181/2003/EC of 13 March 2003. Off J Eur Communities L 71:17
Commission Regulation (1994) Commission regulation 1430/94 of 22 June 1994. Off J Eur Communities L 156:6
Commission Regulation (2010) Commission regulation (EU) no 37/2010 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Off J Eur Communities L 15:1
Council Directive (1996) Council directive 96/23/EC of 29 April 1996 on measures to monitor certain substances and residues thereof in live animals and animal products and repealing directives 85/358/EEC and 86/469/EEC and decisions 89/187/EEC and 91/664/EEC. Off J Eur Commun L 125:10
Fedeniuk RW, McKenzie D, Mizuno M, Neiser C, O’Byrne C, Shurmer B (2015a) Development and validation of determinative and confirmatory LC–MS/MS methodologies for total florfenicol and tulathromycin residues in bovine, equine and porcine kidney, liver and muscle tissues. J Chromatogr B 983–984:1–9
Fedeniuk RW, Mizuno M, Neiser C, O’Byrne C (2015b) Development of LC–MS/MS methodology for the detection/determination and confirmation of chloramphenicol, chloramphenicol 3-O-β-d-glucuronide, florfenicol, florfenicol amine and thiamphenicol residues in bovine, equine and porcine liver. J Chromatogr B 991:68–78
Luo P, Chen X, Liang C, Kuang H, Lu L, Jiang Z, Wang Z, Li C, Zhang S, Shen J (2010) Simultaneous determination of thiamphenicol, florfenicol and florfenicol amine in swine muscle by liquid chromatography–tandem mass spectrometry with immunoaffinity chromatography clean-up. J Chromatogr B 878(2):207–212
Pan X, Wu P, Jiang W, Ma B (2015) Determination of chloramphenicol, thiamphenicol, and florfenicol in fish muscle by matrix solid-phase dispersion extraction (MSPD) and ultra-high pressure liquid chromatography tandem mass spectrometry. Food Control 52:34–38
Power C, Sayers R, Danaher M, Moloney M, O'Brien B, Furey A, Jordan K (2014) Investigation of the persistence of florfenicol residues in bovine milk and fate during processing. Int Dairy J 39(2):270–275
Sadeghi S, Jahani M (2013) Selective solid-phase extraction using molecular imprinted polymer sorbent for the analysis of florfenicol in food samples. Food Chem 141(2):1242–1251
Samanidou V, Galanopoulos L, Kabir A, Furton KG (2015) Fast extraction of amphenicols residues from raw milk using novel fabric phase sorptive extraction followed by high-performance liquid chromatography-diode array detection. Anal Chim Acta 855:41–50
Shen J, Xia X, Jiang H, Li C, Li J, Li X, Ding S (2009) Determination of chloramphenicol, thiamphenicol, florfenicol, and florfenicol amine in poultry and porcine muscle and liver by gas chromatography-negative chemical ionization mass spectrometry. J Chromatogr B 877(14–15):1523–1529
Smith S, Gieseker C, Reimschuessel R, Decker C, Carson MC (2009) Simultaneous screening and confirmation of multiple classes of drug residues in fish by liquid chromatography-ion trap mass spectrometry. J Chromatogr A 1216(46):8224–8232
Tao Y, Zhu F, Chen D, Wei H, Pan Y, Wang X, Liu Z, Huang L, Wang Y, Yuan Z (2014) Evaluation of matrix solid-phase dispersion (MSPD) extraction for multi-fenicols determination in shrimp and fish by liquid chromatography–electrospray ionisation tandem mass spectrometry. Food Chem 150:500–506
Xie K, Jia L, Yao Y, Xu D, Chen S, Xie X, Pei Y, Bao W, Dai G, Wang J, Liu Z (2011) Simultaneous determination of thiamphenicol, florfenicol and florfenicol amine in eggs by reversed-phase high-performance liquid chromatography with fluorescence detection. J Chromatogr B 879(23):2351–2354
Zhang S, Liu Z, Guo X, Cheng L, Wang Z, Shen J (2008) Simultaneous determination and confirmation of chloramphenicol, thiamphenicol, florfenicol and florfenicol amine in chicken muscle by liquid chromatography–tandem mass spectrometry. J Chromatogr B 875(2):399–404
Acknowledgments
The authors would like to thank C. Navarro, C. Gargallo, X. Sáez, M. Lamas and G. Solà for their assistance in the experimental work.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Funding
This study was not funded by any grant.
Conflict of Interest
Francisco Moragues, Carmen Igualada and Nuria León declare that they have no conflict of interest.
Ethical Approval
This article does not contain any studies with human participants or animals performed by any of the authors.
Informed Consent
Not applicable.
Rights and permissions
About this article
Cite this article
Moragues, F., Igualada, C. & León, N. Confirmatory Method for the Determination of Amphenicols in Muscle and Kidney of Several Animal Species. Food Anal. Methods 10, 610–617 (2017). https://doi.org/10.1007/s12161-016-0623-2
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12161-016-0623-2