Determination of zeranol and β-zearalanol in calf urine by immunoaffinity extraction and gas chromatography-mass spectrometry after repeated administration of zeranol

Renzo Bagnati, Maurizio Paleologo Oriundi, Vincenzo Russo, Marisa Danese, Federico Berti, Roberto Fanelli

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Abstract

A method for the determination of zeranol and its metabolite β-zearalanol in bovine urine is described. It has been applied to samples from calves given multiple subcutaneous doses of zeranol. Samples were extracted with immunoaffinity columns containing antibodies raised against zeranol and were analysed by gas chromatography-mass spectrometry. The immunoaffinity columns were prepared by coupling immunoglobulin G fractions obtained from rabbit antisera with a Sepharose matrix. The immunizing agent was carboxybutylzeranol coupled to bovine serum albumin. Gas chromatography-mass spectrometry was performed in the negative-ion chemical ionization mode, after derivatization of the compounds to their pentafluorobenzyl ethers, and allowed detection of analytes with a sensitivity of 0.01 ppb in spiked urine. The derivatization method and the gas chromatographic determination were also applied to the similar compounds zearalanone, zearalenone and β-zearalenol. A synthesis of dideuterated zeranol and β-zearalanol by isotopic exchange is described. These deuterated analogues had an isotopic purity of more than 99% and were used for quantitation of zeranol and β-zearalanol by isotope dilution mass spectrometry. The recoveries of zeranol and β-zearalanol, using the immunoaffinity columns, were determined after extraction from spiked urine and were 84 and 64%, respectively. The urines of treated calves were collected for several days after treatments and were analysed after hydrolysis with β-glucuronidase and arylsulphatase. The samples showed variable but generally decreasing concentrations of zeranol and β-zearalanol. The levels of β-zearalanol ranged from

Original languageEnglish
Pages (from-to)493-502
Number of pages10
JournalJournal of Chromatography B: Biomedical Sciences and Applications
Volume564
Issue number2
DOIs
Publication statusPublished - Apr 5 1991

Fingerprint

Zeranol
Gas chromatography
Gas Chromatography-Mass Spectrometry
Mass spectrometry
Urine
Arylsulfatases
Zearalenone
Ethers
Glucuronidase

ASJC Scopus subject areas

  • Chemistry(all)
  • Clinical Biochemistry
  • Molecular Medicine

Cite this

Determination of zeranol and β-zearalanol in calf urine by immunoaffinity extraction and gas chromatography-mass spectrometry after repeated administration of zeranol. / Bagnati, Renzo; Oriundi, Maurizio Paleologo; Russo, Vincenzo; Danese, Marisa; Berti, Federico; Fanelli, Roberto.

In: Journal of Chromatography B: Biomedical Sciences and Applications, Vol. 564, No. 2, 05.04.1991, p. 493-502.

Research output: Contribution to journalArticle

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abstract = "A method for the determination of zeranol and its metabolite β-zearalanol in bovine urine is described. It has been applied to samples from calves given multiple subcutaneous doses of zeranol. Samples were extracted with immunoaffinity columns containing antibodies raised against zeranol and were analysed by gas chromatography-mass spectrometry. The immunoaffinity columns were prepared by coupling immunoglobulin G fractions obtained from rabbit antisera with a Sepharose matrix. The immunizing agent was carboxybutylzeranol coupled to bovine serum albumin. Gas chromatography-mass spectrometry was performed in the negative-ion chemical ionization mode, after derivatization of the compounds to their pentafluorobenzyl ethers, and allowed detection of analytes with a sensitivity of 0.01 ppb in spiked urine. The derivatization method and the gas chromatographic determination were also applied to the similar compounds zearalanone, zearalenone and β-zearalenol. A synthesis of dideuterated zeranol and β-zearalanol by isotopic exchange is described. These deuterated analogues had an isotopic purity of more than 99{\%} and were used for quantitation of zeranol and β-zearalanol by isotope dilution mass spectrometry. The recoveries of zeranol and β-zearalanol, using the immunoaffinity columns, were determined after extraction from spiked urine and were 84 and 64{\%}, respectively. The urines of treated calves were collected for several days after treatments and were analysed after hydrolysis with β-glucuronidase and arylsulphatase. The samples showed variable but generally decreasing concentrations of zeranol and β-zearalanol. The levels of β-zearalanol ranged from",
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