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Determination of steroid sex hormones in real matrices by bar adsorptive microextraction (BAμE)

In the present work, the development of a novel analytical approach which combines a miniaturized bar adsorptive microextraction device with a micro-liquid desorption in one single step, followed by high performance liquid chromatography with diode array detection (BAµE-µLD/HPLC–DAD), is proposed fo...

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Bibliographic Details
Published in:Talanta (Oxford) 2015-05, Vol.136, p.145-154
Main Authors: Almeida, C., Nogueira, J.M.F.
Format: Article
Language:English
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Summary:In the present work, the development of a novel analytical approach which combines a miniaturized bar adsorptive microextraction device with a micro-liquid desorption in one single step, followed by high performance liquid chromatography with diode array detection (BAµE-µLD/HPLC–DAD), is proposed for the determination of trace levels of nine steroid hormones (estriol, 17ß-estradiol, 17α-estradiol, 19-northisterone, 17α-ethynylestradiol, estrone, d-(-)-norgestrel, progesterone and mestranol) in environmental and biological matrices. From the comparison of ten different coating phases (five polymeric and five activated carbon sorbents), the modified pyrrolidone polymer (P2) showed the best compromise between selectivity and efficiency. Assays performed through BAµE(P2, 1.3mg)-µLD(100µL)/HPLC–DAD on 25mL of ultrapure water samples spiked at the 6.0μg/L level, yielded recoveries ranging from 93±9% to 101±8%, under optimized experimental conditions. The analytical performance showed convenient detection (50.0–100.0ng/L) and quantification limits (165.0–330.0ng/L), as well as good linear dynamic ranges (0.2–24.0µg/L) with remarkable determination coefficients (r2>0.9968). Excellent repeatability were also achieved through intraday (RSD
ISSN:0039-9140
1873-3573
DOI:10.1016/j.talanta.2014.11.013