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Determination of 2‐methoxyestradiol in human plasma, using liquid chromatography/tandem mass spectrometry
Author(s) -
Lakhani Nehal J.,
Lepper Erin R.,
Sparreboom Alex,
Dahut William L.,
Venitz Jürgen,
Figg William D.
Publication year - 2005
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1902
Subject(s) - chemistry , chromatography , calibration curve , extraction (chemistry) , mass spectrometry , liquid chromatography–mass spectrometry , atmospheric pressure chemical ionization , analytical chemistry (journal) , detection limit , chemical ionization , ionization , ion , organic chemistry
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® C 18 column (2.1 × 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. Copyright © 2005 John Wiley & Sons, Ltd.