Determination of zeranol, taleranol, zearalanone, α-zearalenol, β-zearalenol and zearalenone in urine by LC-MS/MS
PBN-AR
Instytucja
Państwowy Instytut Weterynaryjny - Państwowy Instytut Badawczy
Informacje podstawowe
Główny język publikacji
en
Czasopismo
Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
ISSN
1944-0049
EISSN
1944-0057
Wydawca
TAYLOR & FRANCIS LTD
DOI
URL
Rok publikacji
2013
Numer zeszytu
6
Strony od-do
987-994
Numer tomu
30
Identyfikator DOI
Liczba arkuszy
Słowa kluczowe
en
RAL hormones
liquid chromatography
mass spectrometry
Streszczenia
Język
en
Treść
An LC-MS/MS method was developed for the sensitive and selective determination of zeranol, taleranol, zearalanone, α-zearalenol, β-zearalenol and zearalenone in animal urine. Analysis was performed on the free compounds after enzymatic deconjugation. Sample preparation included liquid-liquid extraction followed by solid-phase extraction (SPE) with C18 and NH2 columns. For chromatographic separation of hormones an Inertsil(®) ODS-3 analytical column (150 mm × 2.1 mm, 3 µm) was used. The analytes were determined and identified by LC-MS/MS on a QTRAP5500 instrument with a TurboIon-Spray source operating in negative electrospray ionisation mode. For confirmatory purposes at least two transitions were obtained for each analyte. According to Commission Decision 2002 /657/EC the validation parameters - recovery, repeatability, reproducibility, linearity, specificity, decision limits and detection capabilities - were determined. All parameters were in agreement with 2002/657/EC performance criteria. The apparent recovery ranged from 76.2% to 116.3% for all examined compounds. The repeatability was below 20% and reproducibility did not exceed the limit of 25% for most analytes. Linearity was good for all analytes in the whole range of tested concentrations, as proved by the correlation coefficients greater than 0.99. The decision limits (CCα) ranged from 0.04 to 0.18 μg l(-1) for all analytes whereas the detection capabilities (CCβ) ranged from 0.07 to 0.31 μg l(-1), respectively. All CCα and CCβ values were below the recommended concentration of 2 μg l(-1). This analytical method will be used in an integrated system for Polish monitoring programmes for the confirmation of violative screened samples.
Cechy publikacji
ORIGINAL_ARTICLE
Inne
System-identifier
552325
CrossrefMetadata from Crossref logo
Cytowania
Liczba prac cytujących tę pracę
Brak danych
Referencje
Liczba prac cytowanych przez tę pracę
Brak danych