Evidence map›Paper›PMID 26946022›Full record

ArticleTalanta2016

Derivatization of estrogens enhances specificity and sensitivity of analysis of human plasma and serum by liquid chromatography tandem mass spectrometry.

Abdullah M M Faqehi, Diego F Cobice, Gregorio Naredo, Tracy C S Mak, Rita Upreti, Fraser W Gibb, Geoffrey J Beckett, Brian R Walker, Natalie Z M Homer, Ruth Andrew

Abstract read
In one paragraph

Article in Talanta, 2016. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 29 papers, 1 of them a synthesis that pooled it.

0numbers the graph read from it
0cells of the map it votes in
29citing papers in PubMed, 1 pooled it
–field-weighted citation impact
1 · What the graph read from it

What it found

Each row is one number read from the abstract, on the scale the paper reported it, with its interval. Left of the dashed line favours the treatment, right favours the comparator. Under each row is the sentence it came from. New to these charts? A ten-minute tutorial.

The abstract states no effect estimate the extractor could read, or names no intervention and outcome on the map, so this paper lights no cell and moves no belief. It is still indexed, cited and linked below.

2 · The registry

The trial behind it

Trials whose registry record cites this paper, or whose number appears in the abstract. A trial that started after this paper was published is citing it as background, not reporting it.

Neither the registry nor the abstract names a trial number. If this is a trial report, that itself is worth knowing.

3 · Its place in the literature

Who cites it

29 citing papers in PubMed, 1 synthesis or guideline pooled it.

  1. Pooled it
  2. Aromatase Inhibition Reduces Insulin Sensitivity in Healthy Men.The Journal of clinical endocrinology and metabolism · 2016
    Trial
  3. Article
  4. Review
  5. Article
  6. Review
  7. Article
  8. Article
  9. Article
  10. Article
  11. Article
  12. Article
  13. Stability of sample extracts of vitamin DAnalytical and bioanalytical chemistry · 2023
    Article
  14. Article
  15. Article
  16. Article
  17. Article
  18. LC-HRMS of derivatized urinary estrogens and estrogen metabolites in postmenopausal women.Journal of chromatography. B, Analytical technologies in the biomedical and life sciences · 2020
    Article
  19. Article
  20. Current strategies for quantification of estrogens in clinical research.The Journal of steroid biochemistry and molecular biology · 2019
    Review
4 · The record

Corrections and comments

PubMed lists nothing against this paper. Absence here is not a guarantee, only a check that was made.

5 · Who and what money

Authors and funding

10 authors.

Abdullah M M FaqehiEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: A.M.M.Faqehi@sms.ed.ac.uk.
Diego F CobiceEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: D.F.Cobice@sms.ed.ac.uk.
Gregorio NaredoMass Spectrometry Core, Edinburgh Clinical Research Facility, Queen's Medical Research Institute, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: gnaredo@outlook.com.
Tracy C S MakEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: C.S.mak@sms.ed.ac.uk.
Rita UpretiEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: ritaupreti@yahoo.com.
Fraser W GibbEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: fraser.gibb@ed.ac.uk.
Geoffrey J BeckettClinical Biochemistry, Royal Infirmary of Edinburgh, 51 Little France Crescent, Edinburgh EH16 4SA, United Kingdom. Electronic address: g.j.beckett@ed.ac.uk.
Brian R WalkerEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom; Mass Spectrometry Core, Edinburgh Clinical Research Facility, Queen's Medical Research Institute, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: b.walker@ed.ac.uk.
Natalie Z M HomerMass Spectrometry Core, Edinburgh Clinical Research Facility, Queen's Medical Research Institute, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: n.z.m.homer@ed.ac.uk.
Ruth AndrewEndocrinology, University/British Heart Foundation Centre for Cardiovascular Science, Queen's Medical Research Institute, University of Edinburgh, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom; Mass Spectrometry Core, Edinburgh Clinical Research Facility, Queen's Medical Research Institute, 47 Little France Crescent, Edinburgh EH16 4TJ, United Kingdom. Electronic address: ruth.andrew@ed.ac.uk.

Funding

British Heart Foundation RG-05-008British Heart Foundation RG/11/4/28734Wellcome Trust 090937
6 · The paper itself

Abstract

Estrogens circulate at concentrations less than 20pg/mL in men and postmenopausal women, presenting analytical challenges. Quantitation by immunoassay is unreliable at these low concentrations. Liquid chromatography tandem mass spectrometry (LC-MS/MS) offers greater specificity and sometimes greater sensitivity, but ionization of estrogens is inefficient. Introduction of charged moieties may enhance ionization, but many such derivatives of estrogens generate non-specific product ions originating from the "reagent" group. Therefore an approach generating derivatives with product ions specific to individual estrogens was sought. Estrogens were extracted from human plasma and serum using solid phase extraction and derivatized using 2-fluoro-1-methylpyridinium-p-toluenesulfonate (FMP-TS). Electrospray in positive mode with multiple reaction monitoring using a QTrap 5500 mass spectrometer was used to quantify "FMP" derivatives of estrogens, following LC separation. Transitions for the FMP derivatives of estrone (E1) and estradiol (E2) were compound specific (m/z 362→238 and m/z 364→128, respectively). The limits of detection and quantitation were 0.2pg on-column and the method was linear from 1-400pg/sample. Measures of intra- and inter-assay variability, precision and accuracy were acceptable (<20%). The derivatives were stable over 24h at 10°C (7-9% degradation). Using this approach, E1 and E2, respectively were detected in human plasma and serum: pre-menopausal female serum (0.5mL) 135-473, 193-722pmol/L; male plasma (1mL) 25-111, 60-180pmol/L and post-menopausal female plasma (2mL), 22-78, 29-50pmol/L. Thus FMP derivatization, in conjunction with LC-MS/MS, is suitable for quantitative analysis of estrogens in low abundance in plasma and serum, offering advantages in specificity over immunoassay and existing MS techniques.

Indexed as

AdultAgedAged, 80 and overBenzenesulfonatesChromatography, LiquidEstradiolEstrogensEstroneFemaleHumansMaleMiddle AgedPostmenopausePremenopausePyridinium CompoundsReproducibility of Results2-fluoro-1-methylpyridinium4-toluenesulfonic acidBenzenesulfonatesEstradiolEstrogensEstronePyridinium CompoundsDerivatizationEstradiolEstroneLiquid chromatographyMass spectrometryMethylpyridinium ether

Identifiers

PMID26946022
PMCPMC4791381

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Registered trials

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Read under generation 80e0d062 · epoch 390. Bibliography from PubMed, PubMed Central and OpenAlex; grants from NIH RePORTER; trial links from ClinicalTrials.gov; estimates, votes and beliefs from the OpenQuestion graph.