期刊
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
卷 856, 期 1-2, 页码 156-164出版社
ELSEVIER
DOI: 10.1016/j.jchromb.2007.05.025
关键词
stir bar sorptive extraction; gas chromatography/mass spectrometry; estrone; 17 beta-estradiol; conjugated equine estrogens; urine samples
The development of a sensitive and solvent-free method for the measurement of estrone (E-1) and 17 beta-estradiol (17 beta-E-2) in human urine samples is described. The deconjugated estrogens were derivatized in situ with acetic acid anhydride and the derivatives were extracted directly from the aqueous samples using stir bar sorptive extraction (SBSE). The compounds containing a secondary alcohol function are further derivatized by headspace acylation prior to thermal desorption and gas chromatography/mass spectrometry (GC/MS). A number of experimental parameters, including salt addition, temperature and time, were optimized to increase the recovery of E-1 and 17 beta-E-2 by SBSE. The derivatization reactions were also optimized to obtain the highest yields of the acylated estrogens. Detection limits of 0.02 and 0.03 ng mL(-1) were obtained for E-1 and 17 beta-E-2, respectively. The method was applied to determine the effect of conjugated equine estrogen intake on the excretion of E-1 and 17 beta-E-2 in human urine samples. Increased levels of the endogenous estrogens were detected after administering a standard dose of Premarin to a female volunteer. Routine monitoring of estrogen levels is recommended to avoid a high urinary excretion of E-1 and 17 beta-E-2, nowadays enlisted as endocrine disrupting chemicals (EDCs), during hormone replacement therapy. (C) 2007 Elsevier B.V. All rights reserved.
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