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

被引：30
作者：
Dusi, Guglielmo [1 ]
Gasparini, Mara [1 ]
Curatolo, Michele [1 ]
Assini, Walter [1 ]
Bozzoni, Eros [1 ]
Tognoli, Nadia [1 ]
Ferretti, Enrica [1 ]
机构：
[1] Ist Zooprofilatt Sperimentale Lombardia & Emilia, I-25124 Brescia, Italy
来源：
ANALYTICA CHIMICA ACTA | 2011年 / 700卷 / 1-2期
关键词：
Corticosteroids; Liver; Mass spectrometry; Decision; 2002/657/EC; EXTRACTION; OPTIMIZATION; TISSUES; MS;
D O I：
10.1016/j.aca.2011.01.011
中图分类号：
O65 [分析化学];
学科分类号：
070302 ; 081704 ;
摘要：
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 (CC alpha), detection capability (CC beta) and ruggedness. All the corticosteroids can be detected at a concentration around 1 mu g 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. (C) 2011 Elsevier B.V. All rights reserved.
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页码：49 / 57
页数：9
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