A high-performance liquid chromatography/tandem mass spectrometric screening method for eight synthetic corticosteroids in bovine feces and the simultaneous differentiation between dexamethasone and betamethasone.
A screening method was developed to monitor the illegal use of synthetic corticosteroids in cattle. Diethyl ether extracts from spiked feces samples were cleaned-up by solid phase extraction followed by semipreparative reversed-phase chromatography (RPC). The fraction containing the corticosteroids was derivatized with ethoxyamine hydrochloride. The corresponding ethoximes were separated using silica-based C18 RPC and analyzed on-line in an ion trap mass spectrometer using atmospheric pressure positive chemical ionization. Ethoxime derivatives of dexamethasone and betamethasone were baseline resolved, allowing for the simultaneous mass spectrometric differentiation of both epimers in bovine feces by conventional non-chiral chromatography. At the lowest level tested (1 micro g/kg), corticosteroids (except triamcinolone) could be identified in compliance with the recent European criteria for residue identification. The quantitative performance of the method was best at residue levels > or = 2 micro g/kg.
Laboratory of Residue Analysis, Biomedical Research Institute, Limburgs Universitair Centrum, Universitaire Campus Gebouw C, 3590 Diepenbeek, Belgium. jeanpaul.noben@luc.ac.be
J P
JP
Noben
B
B
Gielen
E
E
Royackers
M
M
Missotten
A
A
Jacobs
J
J
Raus
D000818:Animals; D001507:Beclomethasone / Q000032:analysis; D001623:Betamethasone / Q000032:analysis*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003907:Dexamethasone / Q000032:analysis*; D005243:Feces / Q000737:chemistry*; D005443:Flumethasone / Q000032:analysis; D005938:Glucocorticoids / Q000032:analysis*; D008403:Mass Screening / Q000379:methods; D013058:Mass Spectrometry / Q000379:methods*; D008775:Methylprednisolone / Q000032:analysis; D011239:Prednisolone / Q000032:analysis; D011241:Prednisone / Q000032:analysis; D014221:Triamcinolone / Q000032:analysis
D005938:Glucocorticoids; D014221:Triamcinolone; D003907:Dexamethasone; D001623:Betamethasone; D011239:Prednisolone; D001507:Beclomethasone; D005443:Flumethasone; D011241:Prednisone; D008775:Methylprednisolone