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Application of hyphenated mass spectrometry techniques for the analysis of urinary free glucocorticoids
Author(s) -
Cuzzola Angela,
Petri Antonella,
Mazzini Francesco,
Salvadori Piero
Publication year - 2009
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.4214
Subject(s) - chemistry , chromatography , analyte , derivatization , cortisone , mass spectrometry , urine , glucocorticoid , matrix (chemical analysis) , sample preparation , resolution (logic) , urinary system , medicine , biochemistry , artificial intelligence , computer science
Alteration of levels of glucocorticoids in plasma and urine can be related to several diseases. In particular, the determination of endogenous glucocorticoids in urine has been reported to provide information on cortisol and cortisone status, on the activities of steroid hormone enzymes and on glucocorticoid metabolism. In this study, the application of hyphenated mass spectrometry techniques (GC/MS without derivatization and LC/MS) for the simultaneous analysis of free urinary cortisol (F), cortisone (E), tetrahydrocortisol (THF), allo‐tetrahydrocortisol (A‐THF) and tetrahydrocortisone (THE) was evaluated. A sample preparation protocol by solid‐phase extraction, mass spectrometry parameters and chromatographic conditions for both techniques were carefully optimized in terms of extracting phase and solvents, matrix effects, recovery, sensitivity and compound resolution. Baseline separation was achieved for the five underivatized analytes both in GC and LC. The LC/MS/MS technique was more suitable for the analysis of urine samples, being less influenced by matrix effects and showing excellent sensitivity and selectivity. A preliminary application of the reported method for the diagnosis of metabolic diseases was also described. The determination of each analyte in its free form, described for the first time in the paper, offers new perspectives in the application of glucocorticoid analysis for diagnostic purposes. Copyright © 2009 John Wiley & Sons, Ltd.