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Quantification of 6 Glucocorticoids in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry: Method Development, Validation, and Assessment of Matrix Effects.
MedLine Citation:
PMID:  21743383     Owner:  NLM     Status:  Publisher    
BACKGROUND:: Glucocorticoids are a group of steroid hormones with immunosuppressive and anti-inflammatory properties. In this article, we report the development and the validation of a liquid chromatography tandem mass spectrometry method for the simultaneous quantification of prednisolone, prednisone, cortisol, cortisone, methylprednisolone, and dexamethasone in human plasma. Furthermore, matrix effects were assessed qualitatively and quantitatively. METHODS:: Plasma protein precipitation was performed with acetonitrile containing internal standards. Liquid-liquid extraction with dichloromethane and evaporation were used for cleanup and enrichment. The glucocorticoids were analyzed using reversed-phase chromatography and multiple reaction monitoring of positive ions. RESULTS:: The mean extraction recovery was in the range 66.5%-104.8%, whereas the lower limits of quantification ranged from 1.5 to 4.0 μg/L. The intraday and interday accuracies of all the analytes were within 89.4%-116.6%, and imprecision was <15.6%. Ion suppression ranged from 15.3% to 27.3%. However, the matrix effects did not compromise the assay performance, with mean deviations in calculated concentrations of -4.8% to 2.1% between methanol and matrix. Short-term stability was acceptable for 5 of the analytes, with deviations from baseline between -3.4% and 8.7% after 24 hours at 4°C, although methylprednisolone was stable for 6 hours with a degradation of 10.2%. Deviations from baseline in controls stored at -20°C for 6 months ranged from -22.3% to 6.3%. All analytes were stable after 3 repetitive freeze-thaw cycles, with a maximum degradation of 5.5%. In terms of postpreparative stability, the analytes were stable after 24 and 48 hours at 4°C, with maximum degradation of 6.1% and 9.4%, respectively. CONCLUSIONS:: A validated, sensitive, selective, and reproducible method for quantifying the concentrations of 6 glucocorticoids in human plasma by liquid chromatography tandem mass spectrometry is reported.
Ingjerd Sæves; Nils T Vethe; Stein Bergan
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Publication Detail:
Type:  JOURNAL ARTICLE     Date:  2011-7-02
Journal Detail:
Title:  Therapeutic drug monitoring     Volume:  -     ISSN:  1536-3694     ISO Abbreviation:  -     Publication Date:  2011 Jul 
Date Detail:
Created Date:  2011-7-11     Completed Date:  -     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  7909660     Medline TA:  Ther Drug Monit     Country:  -    
Other Details:
Languages:  ENG     Pagination:  -     Citation Subset:  -    
From the *Department of Medical Biochemistry, Oslo University Hospital, Oslo, Norway; †Department of Pharmaceutical Biosciences, School of Pharmacy, University of Oslo, Oslo, Norway; and ‡Department of Pharmacology, Oslo University Hospital, Oslo, Norway.
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