Development and evaluation of a reference measurement procedure for the determination of total 3,3',5-triiodothyronine in human serum using isotope-dilution liquid chromatography-tandem mass spectrometry
Abstract
3,3',5-Triiodothyronine (T3) is an important diagnostic marker for thyroid function. A reference measurement procedure (RMP) for total T3 in serum involving isotope dilution coupled with liquid chromatography-tandem mass spectrometry (LC/MS/MS) has been developed and critically evaluated. The method uses solid-phase extraction with mixed-mode retention mechanisms of reversed phase and ion exchange prior to reversed-phase LC/MS/MS. In addition to a labeled T3 internal standard (T3-13C9), labeled thyroxine (T4-d5) is also added to serum samples in order to monitor the degradation of T4 to T3. The accuracy of the measurement was evaluated by a recovery study for added T3 and was supported by a comparison study with the other RMP. The recovery of the added T3 ranged from 98.9% to 99.4%. The results of this method and the other RMP agreed to within 1%. Samples of frozen serum pools were prepared and measured in three separate sets. Excellent reproducibility was obtained with within-set coefficients of variation (CVs) ranging from 0.8% to 1.6% and between-set CVs ranging from 1.9% to 2.6%. Excellent linearity was also obtained with correlation coefficients of all linear regression lines (measured intensity ratios vs mass ratios) ranging from 0.9995 to 0.9996. The detection limit at a signal-to-noise ratio of approximately 3 was 1 pg of T3. The T4 degradation during sample preparation was minimized to a small percentage (no more than 3% of the T3 values) by use of antioxidants (asco…
Integrity signals
Registry
Cites
Statistics
Claims the paper makes
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?
Several laboratories have developed procedures to accurately determine total T4 and total T3 in human plasma or serum and largely agree on concentration ranges, but this consensus has not been achieved for most other TH metabolites.
“While meanwhile several laboratories developed procedures to accurately determine total T4 and total T3 in human plasma or serum and largely agree on concentrations ranges (25, 67–73), this consensus has not been achieved yet for most of the other TH metabolites, which occur at much lower concentrations.”
From 3,5-T2—A Janus-Faced Thyroid Hormone Metabolite Exerts Both Canonical T3-Mimetic Endocrine and Intracrine Hepatic Action (2020) · cites this paper as [73]
Cited by
Sorted by citations
Yue, B., Rockwood, A. L., Sandrock, T., La’ulu, S. L., Kushnir, M. M., & Meikle, A. W. (2008) · Clinical Chemistry · doi:10.1373/clinchem.2007.098293 · Cited by 127 · see citing works
Carvalho, V. M. (2012) · Journal of Chromatography B · doi:10.1016/j.jchromb.2011.08.027 · Cited by 90 · see citing works
Köhrle, J., Lehmphul, I., Pietzner, M., Renko, K., Rijntjes, E., Richards, K., Anselmo, J., Danielsen, M., & Jonklaas, J. (2020) · Frontiers in Endocrinology · doi:10.3389/fendo.2019.00787 · Cited by 23 · see citing works
Köhrle, J., & Richards, K. H. (2020) · Experimental and Clinical Endocrinology & Diabetes · doi:10.1055/a-1175-4610 · Cited by 7 · see citing works
- Authors
- Tai, S. S.-C., Bunk, D. M., White, & Welch, M. J.
- Affiliations
- National Institute of Standards and Technology (US)
- Corresponding author
- Tai, Susan S.-C.
- ORCID
- Bunk, David M.
- Venue
- Analytical Chemistry
- Publisher
- American Chemical Society (ACS)
- Published
- 2004-08-05
- Volume
- 76
- Issue
- 17
- Pages
- 5092-5096
- ISSN
- 0003-2700 (ISSN-L)
- 1520-6882
- OpenAlex
- W2094539668
- Cited by
- 88
- References
- 0
- Citations by year
- 2026: 1 · 2025: 4 · 2024: 2 · 2023: 1 · 2022: 2 · 2021: 1 · 2020: 8 · 2019: 2 · 2018: 1 · 2017: 4 · 2016: 5 · 2015: 3 · 2014: 6 · 2013: 5 · 2012: 2
- FWCI
- 2.72
- Type
- journal article
- Language
- en
- Open access
- closed
- Locations
- Analytical Chemistry (publishedVersion)
- PubMed (publishedVersion)
- Funders
- National Institute of Standards and Technology
- Topics
- Health Sciences › Medicine › Endocrinology, Diabetes and Metabolism › Thyroid Disorders and Treatments
- Health Sciences › Medicine › Physiology › Clinical Laboratory Practices and Quality Control
- Social Sciences › Decision Sciences › Statistics, Probability and Uncertainty › Scientific Measurement and Uncertainty Evaluation
- Keywords
- reverse T3, total T3, reference measurement procedure, isotope dilution, liquid chromatography-tandem mass spectrometry, solid-phase extraction, thyroxine to triiodothyronine conversion, human serum, method evaluation, recovery studies
- MeSH terms
- Chromatography, Liquid, Freezing, Humans, Reference Standards, Mass Spectrometry, Triiodothyronine, Reverse, Reproducibility of Results
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
