Determination of 2-methoxyestradiol in human plasma, using liquid chromatography/tandem mass spectrometry

Nehal J. Lakhani, Erin R. Lepper, Alex Sparreboom, William L. Dahut, Jürgen Venitz, William D. Figg*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

29 Scopus citations

Abstract

A liquid chromatography/tandem mass spectrometric (LC/MS/MS) assay was developed for the quantitative determination of 2-methoxyestradiol (2ME2) in human plasma. Sample pretreatment involved liquid-liquid extraction with ethyl acetate of 0.3-mL aliquots of plasma spiked with the internal standard, deuterated 2ME2 (2ME2-d5). Separation was achieved on a Zorbax Eclipse® C18 column (2.1 x 50 mm, i.d., 5 μm) at room temperature using a gradient elution with methanol and water at a flow rate of 0.25 mL/min. Detection was performed using atmospheric pressure chemical ionization MS/MS by monitoring the ion transitions from m/z 303.1 → 136.8 (2ME2) and m/z 308.1 → 138.8 (2ME2-d5). Calibration curves were linear in the concentration range of 1-100 ng/ mL. The accuracy and precision values, obtained from three different sets of quality control samples analyzed in quintuplicate on four separate occasions, ranged from 105-108% and from 3.62-5.68%, respectively. This assay was subsequently used for the determination of 2ME2 concentration in plasma of a patient with cancer after a single oral administration of 2ME2 at a dose of 2200 mg.

Original languageEnglish
Pages (from-to)1176-1182
Number of pages7
JournalRapid Communications in Mass Spectrometry
Volume19
Issue number9
DOIs
StatePublished - 2005
Externally publishedYes

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