A Simple and Rapid LC-MS/MS Method for Determination of Dexamethasone in Bovine Milk
Mehmet Nihat Ural, Arzu Kotan
Abstract
Mehmet Nihat Ural, Arzu Kotan
Abstract
Abstract This study provides insight into the development and validation of the simple, rapid and sensitive method of Liquid Chromatography-Tandem Mass Spectrometry for determining the residues of dexamethasone in bovine milk. The maximum residue limit for dexamethasone in bovine milk is 0.3 ng/ml −1 . Chromatographic separation was achieved on an Agilent Proshell 120 SB:C18 (2.7µm 100x3.0 mm) column. The bovine milk was extracted with ethyl acetate, and the evaporated elution was dissolved with hexane, water and methanol, and analyzed by the LC-MS/MS method. The mobile phase A was a solution of 5 Mm ammonium formate in water, while the mobile phase B was 0.1% formic acid in acetonitrile. The calibration graphics were prepared within the range of 0.15–0.6 ng/ml −1 , and a successful linearity was achieved (r ≥0.999). The limit of detection was 0.016 ng/ml −1 . The decision limit (CCα) and detection capability (CCβ) were 0.34 and 0.38 ng/ml −1 , respectively.
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Abstract This study provides insight into the development and validation of the simple, rapid and sensitive method of Liquid Chromatography-Tandem Mass Spectrometry for determining the residues of dexamethasone in bovine milk. The maximum residue limit for dexamethasone in bovine milk is 0.3 ng/ml −1 . Chromatographic separation was achieved on an Agilent Proshell 120 SB:C18 (2.7µm 100x3.0 mm) column. The bovine milk was extracted with ethyl acetate, and the evaporated elution was dissolved with hexane, water and methanol, and analyzed by the LC-MS/MS method. The mobile phase A was a solution of 5 Mm ammonium formate in water, while the mobile phase B was 0.1% formic acid in acetonitrile. The calibration graphics were prepared within the range of 0.15–0.6 ng/ml −1 , and a successful linearity was achieved (r ≥0.999). The limit of detection was 0.016 ng/ml −1 . The decision limit (CCα) and detection capability (CCβ) were 0.34 and 0.38 ng/ml −1 , respectively.
Key concepts: Chromatography, Ammonium formate, Chemistry, Detection limit, Ammonium acetate, Formic acid, Residue (chemistry), Ethyl acetate