Rapid UHPLC-MS/MS measurement of pregnanediol 3-glucuronide in spot urine samples for detecting ovulation.
LC–MS/MS
dilute and shoot
ovulation
pregnanediol glucuronide
urine
Journal
Biomedical chromatography : BMC
ISSN: 1099-0801
Titre abrégé: Biomed Chromatogr
Pays: England
ID NLM: 8610241
Informations de publication
Date de publication:
16 Aug 2024
16 Aug 2024
Historique:
revised:
23
07
2024
received:
10
06
2024
accepted:
26
07
2024
medline:
16
8
2024
pubmed:
16
8
2024
entrez:
16
8
2024
Statut:
aheadofprint
Résumé
Biochemical confirmation of ovulation typically involves measuring serum progesterone levels during the mid-luteal phase. Alternatively, this information could be obtained by monitoring urinary excretion of conjugated metabolites of ovarian steroids such as pregnanediol 3-glucuronide (PDG) using immunoassay techniques that have methodological limitations. The aim of the present study was to develop a mass spectrometry (MS)-based method for the rapid and accurate measurement of urinary PDG levels in spot urine samples. A "dilute and shoot" ultra-high-performance liquid cromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for measuring PDG urinary concentration with a 6-min analysis time. The method underwent validation in accordance with ISO 17025 documentation for quantitative methods, proving an efficient separation of PDG from other structurally similar glucuro-conjugated steroid metabolites and ensuring a sufficient sensitivity for detecting the target analyte at concentrations as low as 0.01 μg/mL. The validation protocol yielded satisfactory results in terms of accuracy, repeatability, intermediate precision, and combined uncertainty. Additionally, the stability of both the samples and calibration curves was also conducted. The application to real urine samples confirmed the method's capability to measure PDG levels throughout an entire menstrual cycle and detecting ovulation. The rapidity of the analytical platform would therefore enable high throughput analysis, which is advantageous for large cohort clinical studies.
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Pagination
e5982Informations de copyright
© 2024 The Author(s). Biomedical Chromatography published by John Wiley & Sons Ltd.
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