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Simultaneous measurement of endogenous cortisol, cortisone, dehydroepiandrosterone, and dehydroepiandrosterone sulfate in nails by use of UPLC-MS-MS

Identifieur interne : 000A62 ( Main/Exploration ); précédent : 000A61; suivant : 000A63

Simultaneous measurement of endogenous cortisol, cortisone, dehydroepiandrosterone, and dehydroepiandrosterone sulfate in nails by use of UPLC-MS-MS

Auteurs : Mehdi Ben Khelil [France] ; Marion Tegethoff [Suisse, Allemagne] ; Gunther Meinlschmidt [Suisse] ; Carole Jamey [France] ; Bertrand Ludes [France] ; Jean-Sébastien Raul [France]

Source :

RBID : Pascal:11-0405293

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English descriptors

Abstract

Steroid hormone concentrations are mostly determined by using different body fluids as matrices and applying immunoassay techniques. However, usability of these approaches may be restricted for several reasons, including ethical barriers to invasive sampling. Therefore, we developed an ultra-performance LC-MS-MS method for high-throughput determination of concentrations of cortisol, cortisone, dehydroepiandrosterone (DHEA), and DHEA sulfate (DHEAS) in small quantities of human nails. The method was validated for linearity, limits of detection and quantification, recovery, intra and interassay precision, accuracy, and matrix effect. Samples from 10 adult women were analyzed to provide proof-of-principle for the method's applicability. Calibration curves were linear (r2>0.999) in the ranges 10-5000 pg mg-1 for cortisol, cortisone, and DHEAS, and 50-5000 pg mg-1 for DHEA. Limits of quantification were 10 pg mg-1 for cortisol, cortisone, and DHEAS, and 50 pg mg-1 for DHEA. The sensitivity and specificity of the method were good, and there was no interference with the analytes. Mean recovery of cortisol, cortisone, DHEA, and DHEAS was 90.5%, 94.1%, 84.9%, and 95.9%, respectively, with good precision (coefficient of variation <14% for all analytes) and accuracy (relative error (%) -8.3% to 12.2% for all analytes). The median (pg mg-1, range) hormone concentrations were 69.5 (36-158), 65 (32-133), 212 (50-1077), and 246 (115-547) for cortisol, cortisone, DHEA, and DHEAS, respectively. This method enables measurement of cortisol, cortisone, DHEA, and DHEAS in small quantities of human nails, leading to the development of applications in endocrinology and beyond.


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<keywords scheme="KwdEn" xml:lang="en">
<term>Accuracy</term>
<term>Adult</term>
<term>Barrier</term>
<term>Body fluid</term>
<term>Concentration</term>
<term>Detection limit</term>
<term>Endogenous</term>
<term>Human</term>
<term>Immunological method</term>
<term>Interference</term>
<term>Linearity</term>
<term>Liquid chromatography</term>
<term>Mass spectrometry MS/MS</term>
<term>Matrix effect</term>
<term>Measurement method</term>
<term>Performance evaluation</term>
<term>Quantitative analysis</term>
<term>Relative error</term>
<term>Sample</term>
<term>Sampling</term>
<term>Sensitivity</term>
<term>Simultaneous measurement</term>
<term>Specificity</term>
<term>Standard curve</term>
<term>Steroid hormone</term>
<term>Sulfates</term>
<term>Technique</term>
<term>Use</term>
<term>Variation coefficient</term>
</keywords>
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<term>Mesure simultanée</term>
<term>Endogène</term>
<term>Utilisation</term>
<term>Spectrométrie masse tandem</term>
<term>Hormone stéroïde</term>
<term>Concentration</term>
<term>Liquide corporel</term>
<term>Méthode immunologique</term>
<term>Technique</term>
<term>Barrière</term>
<term>Echantillonnage</term>
<term>Evaluation performance</term>
<term>Chromatographie phase liquide</term>
<term>Linéarité</term>
<term>Sulfate</term>
<term>Homme</term>
<term>Limite détection</term>
<term>Analyse quantitative</term>
<term>Précision</term>
<term>Effet matrice</term>
<term>Echantillon</term>
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<term>Courbe étalonnage</term>
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<term>Spécificité</term>
<term>Interférence</term>
<term>Coefficient variation</term>
<term>Erreur relative</term>
<term>Méthode mesure</term>
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<div type="abstract" xml:lang="en">Steroid hormone concentrations are mostly determined by using different body fluids as matrices and applying immunoassay techniques. However, usability of these approaches may be restricted for several reasons, including ethical barriers to invasive sampling. Therefore, we developed an ultra-performance LC-MS-MS method for high-throughput determination of concentrations of cortisol, cortisone, dehydroepiandrosterone (DHEA), and DHEA sulfate (DHEAS) in small quantities of human nails. The method was validated for linearity, limits of detection and quantification, recovery, intra and interassay precision, accuracy, and matrix effect. Samples from 10 adult women were analyzed to provide proof-of-principle for the method's applicability. Calibration curves were linear (r
<sup>2</sup>
>0.999) in the ranges 10-5000 pg mg
<sup>-1</sup>
for cortisol, cortisone, and DHEAS, and 50-5000 pg mg
<sup>-1</sup>
for DHEA. Limits of quantification were 10 pg mg
<sup>-1</sup>
for cortisol, cortisone, and DHEAS, and 50 pg mg
<sup>-1</sup>
for DHEA. The sensitivity and specificity of the method were good, and there was no interference with the analytes. Mean recovery of cortisol, cortisone, DHEA, and DHEAS was 90.5%, 94.1%, 84.9%, and 95.9%, respectively, with good precision (coefficient of variation <14% for all analytes) and accuracy (relative error (%) -8.3% to 12.2% for all analytes). The median (pg mg
<sup>-1</sup>
, range) hormone concentrations were 69.5 (36-158), 65 (32-133), 212 (50-1077), and 246 (115-547) for cortisol, cortisone, DHEA, and DHEAS, respectively. This method enables measurement of cortisol, cortisone, DHEA, and DHEAS in small quantities of human nails, leading to the development of applications in endocrinology and beyond.</div>
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