Development of a multi-class steroid hormone screening method using Liquid Chromatography/Tandem Mass Spectrometry (LC-MS/MS)

Boggs, Ashley S. P.; Bowden, John A.; Galligan, Thomas M.; Guillette, Louis J.; Kucklick, John R.

doi:10.1007/s00216-016-9512-1

Cited by 71Analytical Chemistry and ChromatographyPesticide Residue Analysis and SafetyAnalytical Methods in Pharmaceuticals

Development of a multi-class steroid hormone screening method using Liquid Chromatography/Tandem Mass Spectrometry (LC-MS/MS)

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Boggs, Ashley S. P., Bowden, John A., Galligan, Thomas M., Guillette, Louis J., Kucklick, John R.·2016·Analytical and Bioanalytical Chemistry

DOI 10.1007/s00216-016-9512-1PMC PMC4906791

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Abstract

Monitoring complex endocrine pathways is often limited by indirect measurement or measurement of a single hormone class per analysis. There is a burgeoning need to develop specific direct-detection methods capable of providing simultaneous measurement of biologically relevant concentrations of multiple classes of hormones (estrogens, androgens, progestogens, and corticosteroids). The objectives of this study were to develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for multi-class steroid hormone detection using biologically relevant concentrations, then test limits of detection (LOD) in a high-background matrix by spiking charcoal-stripped fetal bovine serum (FBS) extract. Accuracy was tested with National Institute of Standards and Technology Standard Reference Materials (SRMs) with certified concentrations of cortisol, testosterone, and progesterone. 11-Deoxycorticosterone, 11-deoxycortisol, 17-hydroxypregnenolone, 17-hydroxyprogesterone, adrenosterone, androstenedione, cortisol, corticosterone, dehydroepiandrosterone, dihydrotestosterone, estradiol, estriol, estrone, equilin, pregnenolone, progesterone, and testosterone were also measured using isotopic dilution. Dansyl chloride (DC) derivatization was investigated maintaining the same method to improve and expedite estrogen analysis. Biologically relevant LODs were determined for 15 hormones. DC derivatization improved estrogen response two- to eight-fold, and improved chromatographic separation. All measurements had an accuracy ≤14 % difference from certified values (not accounting for uncertainty) and relative standard deviation ≤14 %. This method chromatographically separated and quantified biologically relevant concentrations of four hormone classes using highly specific fragmentation patterns and measured certified values of hormones that were previously split into three separate chromatographic methods.

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Several sensitive and robust LC-MS/MS methods for multiple steroids have been developed in recent years and many methods meet the requirements for clinical applications.
“Several sensitive and robust LC-MS/MS methods for multiple steroids have been developed in recent years and many methods meet the re quirements for clinical applications [5 -16].”
From Sex- and age-specific reference intervals of 16 steroid metabolites quantified simultaneously by LC-MS/MS in sera from 2458 healthy subjects aged 0 to 77 years (2024) · cites this paper as [6]
The Introduction says LC-MS/MS methods are preferred for direct steroid measurement, and the Results and Discussion describe this paper’s method as effective for measuring several steroid classes. But the Introduction also says many existing multi-class methods have limitations; it does not establish that many methods meet clinical requirements. Page numbers are unavailable in our copy. (LLM, conf=0.85)
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Authors: Boggs, A. S. P., Bowden, J. A., Galligan, T. M., Guillette, L. J., & Kucklick, J. R.
Affiliations: National Institute of Standards and Technology (US)
Medical University of South Carolina (US)
Corresponding author: Boggs, Ashley S. P.
ORCID: Boggs, Ashley S. P.
Bowden, John A.
Galligan, Thomas M.
Kucklick, John R.
Venue: Analytical and Bioanalytical Chemistry
Publisher: Springer Science and Business Media LLC
Published: 2016-04-02
Volume: 408
Issue: 15
Pages: 4179-4190
ISSN: 1618-2642 (ISSN-L)
1618-2650
DOI: 10.1007/s00216-016-9512-1
PMC: PMC4906791
OpenAlex: W2317339084
Cited by: 71
References: 35
Citations by year: 2026: 1 · 2025: 7 · 2024: 6 · 2023: 11 · 2022: 10 · 2021: 5 · 2020: 10 · 2019: 11 · 2018: 7 · 2017: 3
FWCI: 3.49
Type: journal article
Language: en
Open access: green
europepmc.org
Licence: www.springer.com/tdm (tdm)
www.springer.com/tdm (vor)
Locations: Analytical and Bioanalytical Chemistry (publishedVersion)
PubMed (publishedVersion)
Europe PMC (PubMed Central) (acceptedVersion)
PubMed Central (acceptedVersion)
NOAA Institutional Repository (submittedVersion)
Funders: National Research Council
Smart State Center of Economic Excellence for Marine Genomics
National Oceanic and Atmospheric Administration
Topics: Physical Sciences › Chemistry › Spectroscopy › Analytical Chemistry and Chromatography
Life Sciences › Agricultural and Biological Sciences › Food Science › Pesticide Residue Analysis and Safety
Physical Sciences › Chemistry › Analytical Chemistry › Analytical Methods in Pharmaceuticals
Keywords: endocrine monitoring, estrogen, androgens, progestogens, corticosteroids, dansyl chloride derivatization, isotopic dilution, detection limit, fetal bovine serum, cortisol, testosterone, progesterone, estradiol, 17-hydroxypregnenolone, 17-hydroxyprogesterone, adrenosterone, androstenedione, dehydroepiandrosterone, dihydrotestosterone, pregnenolone, equilin, steroid quantification
MeSH terms: Adult, Chromatography, Liquid, Female, Humans, Male, Steroids, Tandem Mass Spectrometry

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Development of a multi-class steroid hormone screening method using Liquid Chromatography/Tandem Mass Spectrometry (LC-MS/MS)

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