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Ultrasonic‐assisted derivatization of estrogenic compounds in a cup horn booster and determination by GC‐MS by Asier Vallejo; Aresatz Usobiaga; Irantzu Martinez‐Arkarazo; Ailette Prieto; Nestor Etxebarria; Olatz Zuloaga; Luis A. Fernández is a Chemistry article available to read on EtoBox.

What is Ultrasonic‐assisted derivatization of estrogenic compounds in a cup horn booster and determination by GC‐MS about?

## Abstract Cup horn boosters are miniaturized ultrasound baths that maximize efficiency and precision. The optimization of an ultrasonic‐assisted derivatization step by means of a cup horn booster and the determination of estrone, 17β‐estradiol, estriol, 17α‐ethynyl estradiol and mestranol was developed by GC‐MS. Different derivatization reagents and solvents were studied for maximizing the di‐derivatization of 17α‐ethynyl estradiol under ultrasound energy. Only __N__,__O__‐__bis__(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane in pyridine gave satisfactory results and this mixture was further used in the optimization of the ultrasound assisted derivatization. The experiment designs included sonication time (1–10 min), sonication power (20–80%), sonication cycles (1–9), derivatization reagent volume (25–125 μL) and solvent volume (25–125 μL). Once the optimum conditions were fixed, the effect of organic matter and the frequency of the water bath change were studied. Finally, the validation of the analytical method was carried out using spiked natural and synthetic waters. Recoveries (natural (138–70%) and synthetic (112–89%)), the LODs (0.35–1.66 ng/L), and LOQ

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Author
Asier Vallejo; Aresatz Usobiaga; Irantzu Martinez‐Arkarazo; Ailette Prieto; Nestor Etxebarria; Olatz Zuloaga; Luis A. Fernández
Publisher
John Wiley and Sons; Wiley (John Wiley & Sons); John Wiley & Sons Ltd.; Wiley (ISSN 1615-9306)
Published
2010
Language
EN
Field
Chemistry (Physical Sciences)

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