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- Title
Sensitive routine liquid chromatography-tandem mass spectrometry method for serum estradiol and estrone without derivatization.
- Authors
Pauwels, Steven; Antonio, Leen; Jans, Ivo; Lintermans, Anneleen; Neven, Patrick; Claessens, Frank; Decallonne, Brigitte; Billen, Jaak; Vanderschueren, Dirk; Vermeersch, Pieter
- Abstract
The need for a routinely applicable assay to measure low estradiol levels in adult men, postmenopausal women, and young adolescents was recently discussed in an Endocrine Society position statement. Our aim was to develop a sensitive liquid chromatography-tandem mass spectrometry method for estradiol and estrone in human serum without the need for derivatization or extended extraction protocols. After protein precipitation of serum with a mixture of methanol/acetonitrile (85/15) ( v/ v) containing isotopic internal standards (17β-estradiol-16,16,17- d and estrone-2,3,4-C), we quantified estradiol and estrone by two-dimensional liquid chromatography-tandem mass spectrometry with electrospray ionization in the negative mode monitoring 5 × 271.20→145.00 (17β-estradiol) and 269.20→145.00 (estrone). Sensitivity was increased by using fluoride and summation of 5 identical transitions for estradiol. Our method was analytically validated, compared against direct immunoassays using serum of 25 adult men, and clinically tested by measuring samples of 3 men at baseline and after chemical castration, 30 postmenopausal women and 15 patients receiving aromatase inhibitors. Total imprecision was below 20 % for the low quality controls. Limit of quantification was 1.3 ng/L (4.8 pmol/L) for estradiol and 1.2 ng/L (4.4 pmol/L) for estrone. Estradiol in Certified Reference Material BCR-576 was within specified uncertainty limits. No significant ion suppression or interference was observed. Our method showed modest correlation with direct immunoassay for estradiol ( r = 0.64) but no correlation for estrone ( r = 0.12). Patient sample results were within expected ranges. In conclusion, we developed a routinely applicable liquid chromatography-tandem mass spectrometry method for estradiol and estrone measurement which is sensitive enough for use in men, postmenopausal women, and young adolescents. [Figure not available: see fulltext.]
- Subjects
LIQUID chromatography-mass spectrometry; ESTRADIOL; ESTRONE; DERIVATIZATION; POSTMENOPAUSE; ELECTROSPRAY ionization mass spectrometry
- Publication
Analytical & Bioanalytical Chemistry, 2013, Vol 405, Issue 26, p8569
- ISSN
1618-2642
- Publication type
Academic Journal
- DOI
10.1007/s00216-013-7259-5