Short Communication
A simple and rapid LC-MS/MS method for determination of dexamethasone in bovine milk
Mehmet Nihat Ural * ,
Arzu Kotan

Mac Vet Rev 2020; 43 (1): 69 - 73

10.2478/macvetrev-2020-0014

Received: 25 September 2019

Received in revised form: 02 January 2020

Accepted: 27 January 2020

Available Online First: 14 February 2020

Published on: 15 March 2020

Correspondence: Mehmet Nihat Ural, nihatural@yahoo.com
PDF HTML

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.

Keywords: dexamethasone, LC-MS/MS, milk

References

  1. Cherlet, M,. De Baere, S., De Backer, P.J. (2004). Quantitative determination of dexamethasone in bovine milk by liquid chromatography-atmospheric pressure chemical ionizationtandem mass spectrometry. J Chromatogr B. 805(1): 57-65. https://doi.org/10.1016/j.jchromb.2004.02.015 PMid:15113540
  2. Van Den Hauwe, O., Schneider, M., Sahin, A., Van Peteghem, C.H., Naegeli, H. (2003). Immunochemical screening and liquid chromatographic−tandem mass spectrometric confirmation of drug residues in edible tissues of calves injected with a therapeutic dose of the synthetic glucocorticoids dexamethasone and flumethasone. J Agric Food Chem. 51(1): 326-330. https://doi.org/10.1021/jf020533m PMid:12502428
  3. Ferranti, C., Famele, M., Palleschi, L., Bozzetta, E., Pezzolato, M., Draisci, R. (2013). Excretion profile of corticosteroids in bovine urine compared with tissue residues after therapeutic and growth-promoting administration of dexamethasone. Steroids 78(9): 803-812. https://doi.org/10.1016/j.steroids.2013.05.002 PMid:23684526
  4. The European Union. Commission Regulation (EU) No 37/2010 of 22 December 2009 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Off J Eur Union L 15:1-72.
  5. De Wasch, K., De Brabander, H., Courtheyn, D., Van Peteghem, C. (1998). Detection of corticosteroids in injection sites and cocktails by MSn. Analyst 123(12): 2415-2422. https://doi.org/10.1039/a804932g PMid:10435271
  6. Hidalgo, O.H., Lopez, M.J., Carazo, E.A., Larrea, MSA., Reuvers, TBA. (2003). Determination of dexamethasone in urine by gas chromatography with negative chemical ionization mass spectrometry. J Chromatogr B. 788(1): 137-146. https://doi.org/10.1016/S1570-0232(02)01039-5
  7. McDonald, M., Granelli, K., Sjöberg, P. (2007). Rapid multi-residue method for the quantitative determination and confirmation of glucocorticosteroids in bovine milk using liquid chromatography-electrospray ionization-tandem mass spectrometry. Anal Chim Acta. 588(1): 20-25. https://doi.org/10.1016/j.aca.2007.01.075 PMid:17386789
  8. Kumar, V., Mostafa, S., Kayo, M.V., Goldberg, E.P., Derendorf, H. (2006). HPLC determination of dexamethasone in human plasma and its application to an in vitro release study from endovascular stents. Pharmazie 61(11): 908-911.
  9. Li, C., Wu, Y., Yang, T., Zhang, Y. (2010). Rapid simultaneous determination of dexamethasone and betamethasone in milk by liquid chromatography tandem mass spectrometry with isotope dilution. J Chromatogr A. 1217(3): 411-414. https://doi.org/10.1016/j.chroma.2009.12.015 PMid:20015503
  10. Croes, K., Goeyens, L., Baeyens, W., Van Loco, J., Impens, S. (2009). Optimization and validation of a liquid chromatography tandem mass spectrometry (LC/MSn) method for analysis of corticosteroids in bovine liver: evaluation of Keyhole Limpet beta-glucuronidase/sulfatase enzyme extract. J Chromatogr B Analyt Technol Biomed Life Sci. 877(7): 635-644. https://doi.org/10.1016/j.jchromb.2009.01.028 PMid:19211313
  11. Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results (2002/657/EC). Off J Eur Commun L221:8-3.
  12. Aerts, M.M.L., Hogenboom, A.C., Brinkman, U.A.T. (1995). Analytical strategies for the screening of veterinary drugs and their residues in edible products. J Chromatogr B Biomed Appl. 667(1): 1-40. https://doi.org/10.1016/0378-4347(95)00021-A  
  13. Malone, E.M., Dowling, G., Elliott, C.T., Kennedy, D.G., Regan, L. (2009). Development of a rapid, multi-class method for the confirmatory analysis of anti-inflammatory drugs in bovine milk using liquid chromatography tandem mass spectrometry. J Chromatogr A. 1216(46): 8132-8140. https://doi.org/10.1016/j.chroma.2009.04.078 PMid:19467664

Copyright

© 2020 Ural M. N. This is an open-access article published under the terms of the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.

Conflict of Interest Statement

The authors have declared that no competing interests exist.

Citation Information

Macedonian Veterinary Review. Volume 43, Issue 1, Pages 69-73, e-ISSN 1857-7415, p-ISSN 1409-7621, DOI: 10.2478/macvetrev-2020-0014, 2020

The all content of the Macedonian Veterinary Review, except where otherwise noted, is licensed under a Creative Commons Attribution License.