CoChat
Sign Up
Cited by 69Stress Responses and CortisolAdrenal Hormones and DisordersAnalytical Methods in Pharmaceuticals

Simultaneous analysis of cortisol and cortisone in saliva using XLC–MS/MS for fully automated online solid phase extraction

Jones, Rachel L., Owen, Laura J., Adaway, Joanne E., Keevil, Brian G.·2012·Journal of Chromatography B
DOI 10.1016/j.jchromb.2011.11.036
Open this paper in CoChat — free account

Abstract

Salivary cortisol measurements are increasingly being used in the investigation of disorders of the hypothalamic-pituitary-adrenal axis. In the salivary gland, cortisol is metabolised to cortisone by the action of 11β-hydroxysteroid dehydrogenase type 2, and cortisone is partly responsible for the variable interference observed in current salivary cortisol immunoassays. The aim of this study was to validate an assay for the simultaneous analysis of salivary cortisol and cortisone using the Spark Holland Symbiosis™ in eXtraction liquid chromatography-tandem mass spectrometry (XLC-MS/MS) mode for fully automated online solid phase extraction (SPE). Saliva samples were diluted in water with the addition of internal standard (d4-cortisol and d7-cortisone). Online SPE was performed using the Spark Holland Symbiosis™ with HySphere™ C18 SPE cartridges and compounds were eluted onto a Phenomenex® C18 guard column attached to a Phenomenex® Onyx monolithic C18 column for chromatography. Mass spectrometry used the Waters® Xevo™ TQ MS in electrospray positive mode. Cortisol and cortisone eluted with their internal standards at 1.95 and 2.17 min, respectively, with a total run time of four minutes. No evidence of ion-suppression was observed. The assay was linear up to 3393 nmol/L for cortisol and 3676 nmol/L for cortisone, with lower limits of quantitation of 0.75 nmol/L and 0.50 nmol/L, respectively. Intra- and inter-assay imprecision was <8.9% for cortisol and <6.5% for cortisone across three levels of internal quality control, with accuracy and recovery within accepted limits. High specificity was demonstrated following interference studies which assessed 29 structurally-related steroids at supra-physiological concentrations. We have successfully validated an assay for the simultaneous analysis of salivary cortisol and cortisone using XLC-MS/MS and fully automated online SPE. The assay benefits from increased specificity compared to immunoassay and minimal sample preparation which allows high sample throughput and is thus suitable for use in a routine clinical laboratory.

Integrity signals

Registry

Crossref · 10.1016/j.jchromb.2011.11.036

Cites

7 of 7 references verified0 citation errors · 0 not checkable

Statistics

Recomputing p-values needs the paper’s full text.

Claims the paper makes

We couldn’t retrieve this paper’s full text, so its claims and self-check weren’t run. The registry and citation checks still apply.

Claims other papers make about this one

Each is checked against this paper’s own text: does it say what the citing paper says it does?

  • Intra-assay coefficients of variation for salivary cortisol and cortisone were less than 9.3% and less than 7.9%; inter-assay CVs were less than 9.7% and less than 10.3% at 1.8 nmol/L to 52.2 nmol/L of salivary cortisol and 3.6 nmol/L to 96 nmol/L of salivary cortisone, respectively.

    “Intra-assay coefficient of variation (CV)s were less than 9.3% and less than 7.9%; and inter-assay CVs were less than 9.7% and less than 10.3% at 1.8 nmol/L to 52.2 nmol/L of salivary cortisol and 3.6 nmol/L to 96 nmol/L of salivary cortisone, respectively [9].”

    From Bioavailability of Oral Hydrocortisone Corrected for Binding Proteins and Measured by LC-MS/MS Using Serum Cortisol and Salivary Cortisone (2018) · cites this paper as [9]

Cites

Flagged first, then by citations

Cited by

Sorted by citations

Authors
Jones, R. L., Owen, L. J., Adaway, J. E., & Keevil, B. G.
Affiliations
  • Wythenshawe Hospital (GB)
  • Manchester Academic Health Science Centre (GB)
Corresponding author
Jones, Rachel L.
ORCID
Venue
Journal of Chromatography B
Publisher
Elsevier BV
Published
2012-01
Volume
881-882
Pages
42-48
ISSN
1570-0232 (ISSN-L)
DOI
10.1016/j.jchromb.2011.11.036
OpenAlex
W1993429674
Cited by
69
References
7
Citations by year
2026: 3 · 2025: 4 · 2024: 3 · 2023: 5 · 2022: 4 · 2021: 3 · 2020: 2 · 2019: 3 · 2018: 6 · 2017: 5 · 2016: 11 · 2015: 6 · 2014: 2 · 2013: 8 · 2012: 4
FWCI
1.74
Type
journal article
Language
en
Open access
closed
Licence
www.elsevier.com/tdm/userlicense/1.0/ (tdm)
Locations
  • Journal of Chromatography B (publishedVersion)
  • PubMed (publishedVersion)
Topics
  • Life Sciences › Neuroscience › Behavioral Neuroscience › Stress Responses and Cortisol
  • Health Sciences › Medicine › Endocrinology, Diabetes and Metabolism › Adrenal Hormones and Disorders
  • Physical Sciences › Chemistry › Analytical Chemistry › Analytical Methods in Pharmaceuticals
Keywords
salivary cortisol, salivary cortisone, 11β-hydroxysteroid dehydrogenase type 2, hypothalamic-pituitary-adrenal axis, clinical laboratory assay
MeSH terms
Chromatography, Liquid, Cortisone, Drug Stability, Humans, Hydrocortisone, Saliva, Sensitivity and Specificity, Reproducibility of Results, Solid Phase Extraction, Tandem Mass Spectrometry

About these checks

Registry, retraction, Cites and statistics results are computed, not judged, with one exception: a printed reference that no index lists is read once by a model before it counts as a citation error. Claims are extracted by a model and kept only when their quote appears verbatim in the text; each cited source is then checked, with a model’s help, for whether it says what the claim relies on. Those verdicts can be wrong — read the claim’s quote and the cited source before relying on one.

Statistics and arithmetic are recomputed, not judged.

Confidence bands are shown only for fields calibrated on our annotated test set. None is calibrated yet, so no band is shown.

What counts as a claim ›How we measure confidence ›How we check this ›

Are you an author, or do you see a problem with this page? Request a review