Preferencje help
Widoczny [Schowaj] Abstrakt
Liczba wyników
2012 | 56 | 3 |

Tytuł artykułu

Determination of zeranol and its metabolites in bovine muscle tissue with gas chromatography-mass spectrometry

Warianty tytułu

Języki publikacji



This paper describes the quantitative method of determination of chosen substances from resorcylic acid lactones group: zeranol, taleranol, α-zearalenol, ß-zearalenol, and zearalanone in bovine muscle tissue. The presented method is based on double diethyl ether liquid-liquid extraction (LLE), solid phase extraction (SPE) clean up, and gas chromatography mass spectrometry (GC- MS) analysis. The residues were derivatised with a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide, ammonium iodide, and DL-dithiothreitol (1,000:2:5, v/w/w). The GC-MS apparatus was operated in positive electron ionisation mode. The method was validated according to the European Union performance criteria pointed in Decision Commission 2002/657/EC. The average recoveries of all analytes at 1 µg kg⁻¹ level were located between 83.7% and 94.5% values with the coefficients of variation values <25%. The decision limits (CCα) and detection capabilities (CCß) for all analytes ranged from 0.58 to 0.82 µg kg⁻¹ and from 0.64 to 0.94 µg kg⁻¹, respectively. The procedure has been accredited and is used as a screening and confirmatory method in control of hormone residues in animal tissues.

Słowa kluczowe








Opis fizyczny



  • Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland


  • 1. ARO SOP 475B, Method validation using ResVal®.Validation according to EC/2002/657, RIVM.
  • 2. Baldwin R.S., Williams R.D., Terry M.K.: Zeranol: a review of the metabolism, toxicology, and analytical methods for detection of tissue residues. Regul Toxicol Pharmacol 1983, 3, 9-25.
  • 3. Blokland M.H., Sterk S.S., Stephany R.W., Launay F.M., Kennedy D.G., Van Ginkel L.A.: Determination of resorcylic acid lactones in biological samples by GC- MS. Discrimination between illegal use and contamination with fusarium toxins. Anal Bioanal Chem 2006, 384, 1221-1227.
  • 4. Chichila T.M.P., Silvestre D., Covey T.R., Henion J.D.: Distribution of zeranol in bovine tissues determined by selected ion monitoring capillary gas chromatography/mass spectrometry. J Anal Toxicol 1988, 12, 310-318.
  • 5. Daeseleire E., Vandeputte R., van Peteghem C.: Validation of multi-residue methods for the detection of anabolic steroids by GC-MS in muscle tissues and urine samples from cattle. Analyst 1998, 123, 2595-2598.
  • 6. Erasmuson A.F., Scahill B.G., West D.M.: Natural zeranol (α-zearalanol) in the urine of pasture-fed animals. J Agr Food Chem 1994, 42, 2721-2725.
  • 7. European Commission SANCO/2004/2726 Guidelines for the implementation of decision 2002/657/EC rev 4- December 2008.
  • 8. European Community Council Directive 96/22/EC of 29 April 1996 concerning the prohibition on the use in stockfarming of certain substances having a hormonal or thyreostatic action and of ß-agonists, and repealing Directives 81/602/EEC, 88/146/EEC and 88/299/EEC. Off J Eur Commun L125:3.
  • 9. European Community 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 L125:10.
  • 10. European Community Commission Decision No. 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretations of results. Off J Eur Commun L221:8.
  • 11. Fang X., Chen J., Gua D., Wang G.: Detection and identification of zeranol in chicken or rabbit liver by liquid chromatography-electrospray tandem mass spectrometry. J AOAC Int 2002, 85, 841-847.
  • 12. ISO/11843: Capability of Detection (Part 1): Terms and Definitions (Part 2): Methodology in the Linear Calibration Case (2000).
  • 13. Jodlbauer J., Zöllner J., Lindner W.: Determination of zeranol, taleranol, zearalenone, α- and ß-zearalenol in urine and tissue by high-performance liquid chromatography-tandem mass spectrometry. Chromatographia 2000, 51, 681-687.
  • 14. Jonker M., Egmond H., Stephany R.W.: CRL-documents 389002096, pp. 39, December 1999.
  • 15. Kennedy D.G., Hewitt S.A., McEvoy J.D.G., Curie J.W., Cannavan A., Blanchflower W.J., Elliot C.T.: Zearalenon is formed from Fusarium spp. toxins in cattle in vivo. Food Addit Contam 1998, 15, 393-400.
  • 16. Launay F.M., Young P.B., Sterk S.S., Blokland M.H., Kennedy D.G.: Confirmatory assay for zeranol, taleranol and the Fusarium spp. toxins in bovine urine using liquid chromatography-tandem mass spectrometry Food Addit Contam 2004, 21, 52-62.
  • 17. McCollum F.T.: Implanting beef calves and stocker cattle. Agricultural Communications 1998, L-2291, No. 4, The Texas A&M University System.
  • 18. Migdalof B.H., Dugger H.A., Heider J.G., Coombs R.A., Terry M.K.: Biotransformation of zeranol: disposition and metabolism in the female rat, rabbit, dog, monkey and man. Xenobiotica 1983, 13, 209-221.
  • 19. Miles Ch.O., Erasmuson A.F., Wilkins A.L., Towers N.R., Smith B.L., Garthwaite I., Scahill B.G., Hansen R.P.: Ovine metabolism of zearalenone to α-zearalanol (zeranol). J Agr Food Chem 1996, 44, 3244-3250.
  • 20. Quintana J.B., Carpinteiro J., Rodríguez I., Lorenzo R.A., Carro A.M., Cela R.: Determination of natural and synthetic estrogens in water by gas chromatography with mass spectrometric detection. J Chromatogr A 2004, 1024, 177-185.
  • 21. Stolker A.A.M., Brinkman U.A.Th.: Analytical strategies for residue analysis of veterinary drugs and growth-promoting agents in food-producing animals-a review. J Chromatogr A 2005, 1067, 15-53.
  • 22. Van Bennekom E.O., Brouwer L., Laurant E.H.M., Hooijering H., Nielen M.W.F.: Confirmatory analysis method for zeranol, its metabolites and related mycotoxin in urine by liquid chromatography-negative ion electrospray tandem mass spectrometry. Anal Chim Acta 2002, 473, 151-160.
  • 23. Vermeire D.A.: Implanting Cattle II: Implant Choices. Baby Doll Nutrition News, 1997, No. 4.
  • 24. Wolthers B.G., Kraan G.P.B.: Clinical aplications of gas chromatography and gas chromatography-mass spectrometry of steroids. J Chromatogr A 1999, 843, 247-274.
  • 25. Woźniak B., Wojtoń B.: Detection of anabolic hormone residues in the urine and muscles of food-producing animals by HPTLC with application of extraction into a solid phase. Bull Vet Inst Pulawy 1996, 40, 55-59.
  • 26. Zöllner P., Jodlbauer J., Kleinova M., Kahlbacher H., Kuhn T., Hochsteiner W., Lindner W.: Concentration levels of zearalenone and its metabolites in urine, muscle tissue, and liver samples of pigs fed with mycotoxin-contaminated oats. J Agr Food Chem 2002, 50, 2494- 2501.

Typ dokumentu



Identyfikator YADDA

JavaScript jest wyłączony w Twojej przeglądarce internetowej. Włącz go, a następnie odśwież stronę, aby móc w pełni z niej korzystać.