Determination of Thyroid Hormones and 11 Metabolites in the Human Serum Using a Simple Derivatization Strategy and Analysis by Isotope-Dilution Liquid Chromatography Tandem Mass Spectrometry

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F65269705%3A_____%2F25%3A00081961" target="_blank" >RIV/65269705:_____/25:00081961 - isvavai.cz</a>

Nalezeny alternativní kódy

RIV/00216224:14310/25:00141102

Výsledek na webu

<a href="https://pubs.acs.org/doi/10.1021/acs.analchem.5c00714" target="_blank" >https://pubs.acs.org/doi/10.1021/acs.analchem.5c00714</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1021/acs.analchem.5c00714" target="_blank" >10.1021/acs.analchem.5c00714</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Determination of Thyroid Hormones and 11 Metabolites in the Human Serum Using a Simple Derivatization Strategy and Analysis by Isotope-Dilution Liquid Chromatography Tandem Mass Spectrometry

Popis výsledku v původním jazyce

Many analytical methods for thyroid hormone (TH) determination lack sensitivity and/or specificity. The thyroid hormone metabolites (THMs) are usually not measured at all. This study describes the development of sensitive high-throughput analytical methods for determining the total concentration and free fraction of TH and THM in the human serum. For the analysis of the TOTAL fraction, we employed protein precipitation and anionic exchanger solid-phase extraction. For the FREE fraction, ultrafiltration and salt-out liquid partitioning were used. Derivatization using dansyl chloride was employed to enhance the sensitivity of HPLC-ESI-MS/MS analysis. Both protocols were validated according to the European Analytical Guidelines (2002/657/EC). We obtained very good recoveries (73-115%) and precision. Interday coefficients of variation (CVs) for most of the analytes ranged from 1.2 to 16.4%. The sensitivity was excellent with detection limits in the sub ppt range for the majority of TH and THM. A significant enhancement in sensitivity (&gt;10 fold) was achieved through derivatization. The applicability was proved on a set of samples from pregnant women enrolled in the CELSPAC cohort (n = 120). Our TH reference ranges are in good agreement with those reported in the literature. The methods also allowed us to quantify the levels of 11 THM, including some previously undetected THM in total and free fractions, and proved to be suitable for high-throughput routine TH and THM analyses. Our approach offers an important advancement in thyroid hormone analysis. To the best of our knowledge, it is for the first time that data for T1A and T2A as well as for free THM levels in the human serum are published in the literature. Moreover, our study also brings the first information about the levels of most of the THM in pregnant women.

Název v anglickém jazyce

Determination of Thyroid Hormones and 11 Metabolites in the Human Serum Using a Simple Derivatization Strategy and Analysis by Isotope-Dilution Liquid Chromatography Tandem Mass Spectrometry

Popis výsledku anglicky

Many analytical methods for thyroid hormone (TH) determination lack sensitivity and/or specificity. The thyroid hormone metabolites (THMs) are usually not measured at all. This study describes the development of sensitive high-throughput analytical methods for determining the total concentration and free fraction of TH and THM in the human serum. For the analysis of the TOTAL fraction, we employed protein precipitation and anionic exchanger solid-phase extraction. For the FREE fraction, ultrafiltration and salt-out liquid partitioning were used. Derivatization using dansyl chloride was employed to enhance the sensitivity of HPLC-ESI-MS/MS analysis. Both protocols were validated according to the European Analytical Guidelines (2002/657/EC). We obtained very good recoveries (73-115%) and precision. Interday coefficients of variation (CVs) for most of the analytes ranged from 1.2 to 16.4%. The sensitivity was excellent with detection limits in the sub ppt range for the majority of TH and THM. A significant enhancement in sensitivity (&gt;10 fold) was achieved through derivatization. The applicability was proved on a set of samples from pregnant women enrolled in the CELSPAC cohort (n = 120). Our TH reference ranges are in good agreement with those reported in the literature. The methods also allowed us to quantify the levels of 11 THM, including some previously undetected THM in total and free fractions, and proved to be suitable for high-throughput routine TH and THM analyses. Our approach offers an important advancement in thyroid hormone analysis. To the best of our knowledge, it is for the first time that data for T1A and T2A as well as for free THM levels in the human serum are published in the literature. Moreover, our study also brings the first information about the levels of most of the THM in pregnant women.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

10406 - Analytical chemistry

Projekt

<a href="/cs/project/EF16_027%2F0008360" target="_blank" >EF16_027/0008360: Postdoc@MUNI</a><br>

Návaznosti

I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Rok uplatnění

2025

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název periodika

Analytical Chemistry

ISSN

0003-2700

e-ISSN

1520-6882

Svazek periodika

97

Číslo periodika v rámci svazku

17

Stát vydavatele periodika

US - Spojené státy americké

Počet stran výsledku

9

Strana od-do

9438-9446

Kód UT WoS článku

001473794400001

EID výsledku v databázi Scopus

2-s2.0-105003382817