Accelerated solvent extraction and liquid chromatography-tandem mass spectrometry quantitation of corticosteroid residues in bovine liver.
A new method for the rapid extraction and unequivocal confirmation of two highly potent fluorinated synthetic corticosteroids, dexamethasone and its beta-epimer betamethasone, in bovine liver was developed. Flumethasone was used as internal standard. An extraction procedure using an accelerated solvent extraction system was employed for the isolation of the analytes in liver samples. The procedure was highly automated, including defatting and extraction steps, sequentially carried out under 1.0 x 10(4) kPa in about 35 min. The extracts were then directly analysed by tandem mass spectrometry with on-line liquid chromatography. The analytes were ionised in a heated nebulizer interface operating in the negative ion mode where the molecular related ions [M-H-CH2O]- were generated for each analyte, at m/z 361 for betamethasone and dexamethasone and at m/z 379 for flumethasone. They served as precursor ions for collision-induced dissociation and three diagnostic product ions for the drugs were identified to carry out analyte confirmation by selected reaction monitoring. Assessment of recovery, specificity and precision for betamethasone, dexamethasone and flumethasone proved the method suitable for confirmatory purposes. The limit of quantification of betamethasone and dexamethasone in liver tissue was 1.0 microg/kg.
Draisci
R
R
Laboratorio Medicina Veterinaria, Istituto Superiore di Sanità, Rome, Italy. draisci@iss.it
Marchiafava
C
C
Palleschi
L
L
Cammarata
P
P
Cavalli
S
S
D000818:Animals; D001623:Betamethasone / Q000032:analysis*; D002138:Calibration; D002417:Cattle; D002853:Chromatography, Liquid / Q000379:methods*; D003907:Dexamethasone / Q000032:analysis*; D004350:Drug Residues / Q000032:analysis*; D005443:Flumethasone / Q000032:analysis*; D005938:Glucocorticoids / Q000032:analysis*; D008099:Liver / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012997:Solvents
D005938:Glucocorticoids; D012997:Solvents; D003907:Dexamethasone; D001623:Betamethasone; D005443:Flumethasone