Confirmational analysis of beta-agonists by cryotrapping GC-FTIR
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Open Access
Type
Report
Language
en
Date
1996-02-29
Research Projects
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Journal Issue
Title
Confirmational analysis of beta-agonists by
cryotrapping GC-FTIR
Translated Title
Bevestigd in 1995 analyse van beta-agonisten met
toepassing van cryotrapping GC-FTIR
Published in
Abstract
Onderzoek is verricht naar de toepasbaarheid van
cryotrapping gaschromatografie-Fourier transform infrarood spectrometrie
(GC-FTIR) als bevestigingsmethode bij de 'selected ion' GC-MS analyse van
beta-agonisten in monsters kalfslever en urine. Clenbuterol, Salbutamol,
Mabuterol, Bromobuterol, Cimaterol, Cimbuterol en Mapenterol werden
gedetecteerd als trimethylsilyl- en als methylboronzuur derivaten. Gebruik
van methylboronzuur als derivatiseringsreagens leidt voor zowel standaarden
als monsterextracten tot een aanzienlijke verlaging van de chemische
achtergrond in de GC-FTIR chromatogrammen. De identificatiegrens van de
methode voor methylboron-zuur gederivatiseerde beta-agonisten is circa 1
nanogram per microliter geinjecteerd extract, hetgeen overeenkomt met 3-8
ppb in het oorspronkelijke monster. De overeenkomst tussen analyt- en
referentiespectrum, in combinatie met de retentietijd, is een bruikbaar
bevestigingscriterium.
Cryotrapping gas chromatography-Fourier transform infrared spectrometry has been used for confirmatory analysis of the beta-agonists Clenbuterol, Salbutamol, Mabuterol, Bromobuterol, Cimaterol, Cimbuterol and Mapenterol in samples of calf urine and liver following gas chromatography-selected ion detection mass spectrometry. Samples were analysed for their trimethylsilyl- and methylboronate-derivatives. Methylboronate derivatization yielded strongly diminished chemical background and interference levels in the IR chromatograms of both standard and sample extracts. The limit of identification for methylboronate derivatives is approximately 1 ng/mul in extracts, which corresponds to 3-8 ppb in incurred samples. The similarity of analyte and reference spectra, together with the retention time, are useful criteria for confirmation.
Cryotrapping gas chromatography-Fourier transform infrared spectrometry has been used for confirmatory analysis of the beta-agonists Clenbuterol, Salbutamol, Mabuterol, Bromobuterol, Cimaterol, Cimbuterol and Mapenterol in samples of calf urine and liver following gas chromatography-selected ion detection mass spectrometry. Samples were analysed for their trimethylsilyl- and methylboronate-derivatives. Methylboronate derivatization yielded strongly diminished chemical background and interference levels in the IR chromatograms of both standard and sample extracts. The limit of identification for methylboronate derivatives is approximately 1 ng/mul in extracts, which corresponds to 3-8 ppb in incurred samples. The similarity of analyte and reference spectra, together with the retention time, are useful criteria for confirmation.
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