Journal
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
Volume 41, Issue 4, Pages 1303-1311Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jpba.2006.02.037
Keywords
stir bar sorptive extraction; HPLC/DAD; endocrine disrupters; steroid sex hormones; estrogens; water analysis; urine matrices; trace analysis
Categories
Ask authors/readers for more resources
In this study, stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-HPLC/DAD) were combined for the simultaneous determination of nine steroid sex hormones (estrone, 17 alpha-estradiol, 17 beta-estradiol, 17 alpha-ethynylestradiol, diethylstilbestrol, mestranol, progesterone, 19-norethisterone and norgestrel) in water and urine matrices. During the method development, it has been demonstrated that equilibrium time, ionic strength and back extraction solvents are the most important parameters to control, for determining the nine-hormones in water matrices, in which stir bars coated with 126 111 of polydimethylsiloxane were used. Assays performed on 30 ml water samples spiked at 10 mu g/l levels under optimised experimental conditions, yielded recoveries ranging from 11.1 +/- 4.9% (17 beta-estradiol) to 100.2 +/- 10.4% (mestranol), showed that the methodology is well described by the octanol-water partition coefficients (K-PDMS/W approximate to K-O/W) for the latter, while pronounced deviations to the theoretical efficiency (KPDMS/W 0 KO/W) were observed for the remaining hormones. From calibration studies, a good analytical performance for all hormones was attained, including a suitable precision (2.1-17.1 %), low limits of detection (0.3-1.0 mu g/l) and an excellent linear dynamic range (1.25-50.0 mu g/l). Assays on environmental water and urine matrices showed recovery yields in worthy good agreement with the spiking level (10 mu g/l), and suitability for profiling low mu g/l levels of natural hormones in urine samples taken from pregnant women. The present methodology is easy, reliable and sensitive at the trace level, only requiring a low samplevolume, showing to be a good analytical alternative to routine quality control for environmental and biomedical laboratories. (c) 2006 Elsevier B.V. All rights reserved.
Authors
I am an author on this paper
Click your name to claim this paper and add it to your profile.
Reviews
Recommended
No Data Available