Towards the non-invasive determination of estradiol levels: Development and validation of an LC-MS/MS assay for quantification of salivary estradiol at sub-pg/mL level.

Autor: Fabregat-Safont D; Applied Metabolomics Research Group, Hospital Del Mar Research Institute, Barcelona, Spain; Environmental and Public Health Analytical Chemistry, Research Institute for Pesticides and Water (IUPA), Univ. Jaume I, Castelló, Spain., Alechaga É; Applied Metabolomics Research Group, Hospital Del Mar Research Institute, Barcelona, Spain., Haro N; Applied Metabolomics Research Group, Hospital Del Mar Research Institute, Barcelona, Spain., Gomez-Gomez À; Applied Metabolomics Research Group, Hospital Del Mar Research Institute, Barcelona, Spain., Velasco ER; Institut de Neurociències, Universitat Autònoma de Barcelona, Cerdanyola Del Vallès, Barcelona, Spain., Nabás JF; Institut de Neurociències, Universitat Autònoma de Barcelona, Cerdanyola Del Vallès, Barcelona, Spain., Andero R; Institut de Neurociències, Universitat Autònoma de Barcelona, Cerdanyola Del Vallès, Barcelona, Spain; Departament de Psicobiologia I de Metodologia de Les Ciències de La Salut, Universitat Autònoma de Barcelona, Cerdanyola Del Vallès, Barcelona, Spain; Centro de Investigación Biomédica en Red de Salud Mental (CIBERSAM), Spain; Unitat de Neurociència Traslacional, Parc Taulí Hospital Universitari, Institut D'Investigació I Innovació Parc Taulí (I3PT), Spain; ICREA, Barcelona, Spain., Pozo OJ; Applied Metabolomics Research Group, Hospital Del Mar Research Institute, Barcelona, Spain. Electronic address: opozo@researchmar.net.
Jazyk: angličtina
Zdroj: Analytica chimica acta [Anal Chim Acta] 2024 Dec 01; Vol. 1331, pp. 343313. Date of Electronic Publication: 2024 Oct 09.
DOI: 10.1016/j.aca.2024.343313
Abstrakt: Background: Estradiol (E2) is a female sex hormone involved in several biological processes. Although E2 levels are commonly measured in blood samples, the use of non-invasive techniques (e.g. determination of salivary E2) would allow for the collection of repeated samples and the inclusion of a greater number of participants. Immunoassay-based techniques to measure salivary E2 failed to accurately mirror the variations observed in the plasmatic concentrations of E2 during the menstrual cycle probably due to the high sensitivity required (in the sub-pg/mL range). Therefore, sensitive and rugged analytical methods for the determination of salivary E2 are required. For this, we developed and validated an analytical methodology for the accurate determination of salivary E2.
Results: The method is based on chemical derivatization with 1,2-dimethyl-1H-imidazole-5-sulphonyl chloride and liquid chromatography-tandem mass spectrometry analysis by summing highly-specific SRM transitions. This strategy allowed for increasing the sensitivity of the method. The validation of the method showed an accurate and precise quantification of E2 in 1 mL of saliva even at 250 fg/mL (97 % accuracy and 15 % RSD intra-day, and 104 % accuracy and 18 % RSD inter-day). In order to evaluate its efficacy, we analysed saliva samples from 5 healthy female volunteers collected during a whole menstrual cycle. Our analyses showed that the variations in the concentration of E2 in the measured samples mirrored those expected during a complete menstrual cycle. Additionally, we validated the suitability of our method for determining salivary E2 levels during pregnancy.
Significance: To the best of our knowledge, this is the first method that allows to precisely and accurately measuring E2 in saliva samples along the whole menstrual cycle of healthy females. It is also suitable for the determination of estradiol during pregnancy. Its high sensitivity makes this strategy ideal for the evaluation of the role of hormone production in women's health.
Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: David Fabregat reports financial support was provided by European Union. Raul Andero reports financial support was provided by European Union. Raul Andero reports financial support was provided by Alicia Koplowitz Foundation. Raul Andero reports financial support was provided by Fundación BBVA. Raul Andero reports financial support was provided by Ministry of Science Technology and Innovations. Raul Andero reports financial support was provided by LaCaixa Foundation. If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
(Copyright © 2024. Published by Elsevier B.V.)
Databáze: MEDLINE
Externí odkaz: