Journal
MICROCHEMICAL JOURNAL
Volume 115, Issue -, Pages 70-77Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.microc.2014.02.012
Keywords
beta-agonists; Bovine urine; UPLC-MS/MS; Solid phase extraction; Validation
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Ultra performance liquid chromatography (UPLC) hyphenated to tandem mass spectrometry (MS/MS) was used for the development of an analytical method capable of simultaneous identification and quantification of 18 beta-agonist compounds namely, brombuterol, chlorbrombuterol, cimaterol, cimbuterol, clenbuterol, clencyclohexerol, clenisopenterol, clenpenterol, clenproperol, hydroxymetylclenbuterol, isoxsuprine, mabuterol, mapenterol (clenbuterol-like compounds), ractopamine, ritodrine, salbutamol, salmeterol (salbutamol-like compounds) and zilpaterol in bovine urine. In compliance with the Commission Decision 2002/657/EC (CD 2002/657/EC), the method was validated applying a matrix-comprehensive in-house validation approach based on a fractional factorial design. Six experimental factors varied on two levels were selected for this purpose. The relevant validation parameters such as decision limit CC alpha (range, 0.24-0.51 mu g L-1) and detection capability cc beta (range, 0.27-0.71 mu g L-1), within-laboratory reproducibility (<20%) as well as recovery (range, 92-109%) were in agreement with the performance criteria set in the CD 2002/657/EC. Overall, the proposed method enabled both screening and confirmatory detection of the beta-agonist compounds in the framework of official monitoring plans. (C) 2014 Elsevier B.V. All rights reserved.
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