Περίληψη:
A robust and sensitive methodology, utilizing GC-MS, for the identification and quantitation of seven β-agonist residues (mabuterol, clenbuterol, brombuterol, mapenterol, clenpenterol, clenproperol, and clencyclohexerol), in liver and meat samples, is described. Different extraction procedures, followed by GC/MS measurement, were tested and compared in order to achieve optimum extraction conditions and eliminate matrix effects. The optimized method consisted of consecutive extractions with hydrochloric tris(hydroxymethyl)aminomethane (TRIS-HCl) and tert-butyl-methyl ether (TBME), defatting with hexane and solid-phase extraction (SPE) with C18 cartridges. Ν,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) with 1% trimethylchlorosilane (TMCS) was used as a derivatization agent and the GC-EI-MS determination was performed using a MDN-5S capillary column in single-ion monitoring (SIM) acquisition mode. The method was validated according to the Commission Decision 2002/657/EC, fulfilling all the EU criteria. Quantification was performed via internal standard calibration using deuterated analogs of the compounds. Recoveries ranged from 83 to 118% (mabuterol at concentration levels of 2.0 and 1.5 μg kg−1, respectively) and precision, expressed as %relative standard deviation (% RSD), was in every case lower than the % RSDs obtained from Horwitz equation. The obtained decision limit (CCα) and detection capability (CCβ) values varied from 0.21 ng g−1 (clenbuterol) to 0.49 ng g−1 (clenproperol, clencyclohexerol) and from 0.60 (mapenterol) to 0.69 ng g−1 (clenpenterol), respectively. © 2018, Springer Science+Business Media, LLC, part of Springer Nature.
Συγγραφείς:
Karamolegou, F.
Dasenaki, M.
Belessi, V.
Georgakilas, V.
Thomaidis, N.
Λέξεις-κλειδιά:
Essential oils; Extraction; Liver; Mass spectrometry; Meats; Phase separation, Bis(trimethylsilyl)trifluoroacetamide; Commission Decision 2002/657/EC; Gas chromatography-mass spectrometry; GC-MS; Multi-residue determination; Optimum extraction conditions; Relative standard deviations; Trishydroxymethylaminomethane, Gas chromatography
