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    Confirmational analysis of beta-agonists by cryotrapping GC-FTIR

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    Authors
    Vredenbregt MJ
    Visser T
    Jong APJM de
    Rossum HJ van
    Stephany RW
    Ginkel LA van
    Type
    Report
    Language
    en
    
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    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
    Publiekssamenvatting
    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.
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    http://hdl.handle.net/10029/257826
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