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Quantitative screening for steroids in animal feeding water using reversed phase LC with gradient elution
Author(s) -
MuñizValencia Roberto,
GonzaloLumbreras Raquel,
SantosMontes Ana,
IzquierdoHornillos Roberto
Publication year - 2008
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700382
Subject(s) - chromatography , repeatability , elution , chemistry , reproducibility , gradient elution , solid phase extraction , high performance liquid chromatography , sample preparation , extraction (chemistry) , analytical chemistry (journal)
Several isocratic separations for the determination of 20 steroids (STER) in animal feeding water samples (AFWS) from drinking‐trough by LC using a mobile phase ACN/H 2 O (35:65 v/v) and different RP columns (Hypersil C18, Gemini C18 (GM), Purospher Star C18, Synergi Max C12, and Synergi Fusion) and UV detection were obtained. The elution order was the same: a first group of corticoids (CC) was early eluted, a second group of CC and anabolics (AAS) exhibited intermediate retention, and a third group constituted by AAS was strongly retained. To improve the separation performances of the isocratic separations an ACN gradient elution optimization was carried out for each column. The most satisfactory results were obtained using a Purospher column which allowed the separation of 19 STER in an analysis time close to 26 min. After sample preparation using SPE, method validation was performed in an AFWS spiked with STER according to the EC decision criteria established for quantitative screening methods. For this purpose calibration graphs, extraction efficiencies, decision limits, detection capabilities, precision (repeatability and within‐laboratory reproducibility), accuracy, selectivity, and robustness were evaluated. The proposed method was applied to other AFWS with satisfactory results.