Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of nine corticosteroid residues in bovine liver samples

Dusi, Guglielmo; Gasparini, Mara; Curatolo, Michele; Assini, Walter; Bozzoni, Eros; Tognoli, Nadia; Ferretti, Enrica (2011). Development and validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous determination of nine corticosteroid residues in bovine liver samples. Analytica Chimica Acta, 700(1-2), pp. 49-57. Amsterdam: Elsevier 10.1016/j.aca.2011.01.011

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A liquid chromatography tandem mass spectrometry (LC-MS/MS) confirmatory method for the simultaneous determination of nine corticosteroids in liver, including the four MRL compounds listed in Council Regulation 37/2010, was developed. After an enzymatic deconjugation and a solvent extraction of the liver tissue, the resulting solution was cleaned up through an SPE Oasis HLB cartridge. The analytes were then detected by liquid chromatography-negative-ion electrospray tandem mass spectrometry, using deuterium-labelled internal standards. The procedure was validated as a quantitative confirmatory method according to the Commission Decision 2002/657/EC criteria. The results showed that the method was suitable for statutory residue testing regarding the following performance characteristics: instrumental linearity, specificity, precision (repeatability and intra-laboratory reproducibility), recovery, decision limit (CCα), detection capability (CCβ) and ruggedness. All the corticosteroids can be detected at a concentration around 1 μg kg(-1); the recoveries were above 62% for all the analytes. Repeatability and reproducibility (within-laboratory reproducibility) for all the analytes were below 7.65% and 15.5%, respectively.

Item Type:

Journal Article (Original Article)

Division/Institute:

04 Faculty of Medicine > Department of Intensive Care, Emergency Medicine and Anaesthesiology (DINA) > Clinic and Policlinic for Anaesthesiology and Pain Therapy

UniBE Contributor:

Curatolo, Michele

ISSN:

0003-2670

Publisher:

Elsevier

Language:

English

Submitter:

Jeannie Wurz

Date Deposited:

04 Oct 2013 14:19

Last Modified:

23 Jan 2018 12:16

Publisher DOI:

10.1016/j.aca.2011.01.011

PubMed ID:

21742116

Web of Science ID:

000293428900008

URI:

https://boris.unibe.ch/id/eprint/6074 (FactScience: 210968)

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