Simultaneous determination of betamethasone and dexamethasone residues in bovine liver by liquid chromatography/tandem mass spectrometry.
In this study a new method for the simultaneous confirmation of betamethasone and dexamethasone residues in bovine liver is presented. A Quattro LCZ triple quadrupole mass spectrometer, equipped with an atmospheric pressure ionization (API) source, was coupled to a high performance liquid chromatograph (HPLC) system. Spiked liver samples were first extracted with acetonitrile, and the extracts were purified on C-18 columns. LC separations were performed on a Hypercarb column, with acetonitrile/water (90:10, v/v, +0.3% formic acid) as the mobile phase. Retention times for dexa- and betamethasone were 6.60 and 8.50 min, respectively. Fluorometholone had a retention time of 6.70 min and was used as the internal standard. The detection of the analytes was performed in the multiple reaction monitoring (MRM) mode. The assay was linear over the range of 0.5 to 8 microg/kg for both analytes. The estimated determination limits were 0.2 microg/kg for both beta- and dexamethasone and the quantification limits were 0.4 microg/kg for dexamethasone and 0.3 microg/kg for betamethasone. Analysis precision at 1, 2 and 4 microg/kg was lower than 6.1% (relative standard deviation, RSD) and accuracy was at least 97.5%. Recoveries at 1, 2 and 4 microg/kg ranged between 56 and 69%.
Van Den Hauwe
O
O
Laboratory of Food Analysis, Faculty of Pharmaceutical Sciences, Ghent University, Harelbekestraat 72, 9000 Ghent, Belgium.
Perez
J C
JC
Claereboudt
J
J
Van Peteghem
C
C
D000818:Animals; D001623:Betamethasone / Q000032:analysis*; D002417:Cattle; D002851:Chromatography, High Pressure Liquid; D002853:Chromatography, Liquid / Q000379:methods*; D003907:Dexamethasone / Q000032:analysis*; D005506:Food Contamination; D005938:Glucocorticoids / Q000032:analysis*; D008099:Liver / Q000737:chemistry*; D013058:Mass Spectrometry / Q000379:methods*; D012680:Sensitivity and Specificity
D005938:Glucocorticoids; D003907:Dexamethasone; D001623:Betamethasone