Determination of α-and β-boldenone sulfate, glucuronide and free forms, and androstadienedione in bovine urine using immunoaffinity columns clean-up and liquid chromatography tandem mass spectrometry analysis
Articolo
Data di Pubblicazione:
2015
Citazione:
Determination of α-and β-boldenone sulfate, glucuronide and free forms, and androstadienedione in bovine urine using immunoaffinity columns clean-up and liquid chromatography tandem mass spectrometry analysis / L. Chiesa, R. Pavlovic, G. Dusi, E. Pasquale, A. Casati, S. Panseri, F. Arioli. - In: TALANTA. - ISSN 0039-9140. - 131(2015 Jan), pp. 163-169. [10.1016/j.talanta.2014.07.035]
Abstract:
The debate about the origins of boldenone in bovine urine is ongoing for two decades in Europe. Despite
the fact that its use as a growth promoter has been banned in the European Union (EU) since 1981, its
detection in bovine urine, in the form of α‐boldenone conjugate, is considered fully compliant up to 2 ng
mL−1. The conjugated form of β‐boldenone must be absent. In recent years, the literature about boldenone
has focused on the identification of biomarkers that can indicate an illicit treatment. β‐boldenone sulfate is
a candidate molecule, even if the only studies currently available have taken place in small populations. In
this study, a method for the determination of sulfate and glucuronate conjugates of β‐boldenone was
developed and validated according to the European Commission Decision 2002/657/EC and applied to α‐
boldenone sulfate and glucuronide, α‐ and β‐boldenone free forms and androstadienedione (ADD), too.
The clean‐up with immunoaffinity columns enabled the direct determination of the conjugates and free
forms and allowed specific and sensitive analyses of urine samples randomly selected to verify this method.
The decision limits (CCα) ranged between 0.07 and 0.08 ng mL−1, the detection capabilities (CCβ) between
0.08 and 0.1 ng mL−1. Recovery was higher than 92% for all the analytes. Intra‐day repeatability was
between 5.8% and 17.2%, and inter‐day repeatability was between 6.0% and 21.8% for the studied free and
conjugated forms. This method has been developed as a powerful tool with the aim to study the origin of
boldenone in a trial on a significant number of animals.
Tipologia IRIS:
01 - Articolo su periodico
Keywords:
Androstadienedione; Boldenone; Boldenone glucuronide; Boldenone sulphate; Bovine urine; Food safety
Elenco autori:
L. Chiesa, R. Pavlovic, G. Dusi, E. Pasquale, A. Casati, S. Panseri, F. Arioli
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