Home Physical Sciences Liquid Chromatography with Fluores-cence Detection as a Tool for Separation of Endocrine Disrupting Alkylphenols and their Mono- and Diethoxylates in Analysis of River Water Samples
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Liquid Chromatography with Fluores-cence Detection as a Tool for Separation of Endocrine Disrupting Alkylphenols and their Mono- and Diethoxylates in Analysis of River Water Samples

  • A. Zgoła-Grześkowiak and T. Grześkowiak
Published/Copyright: April 2, 2013
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Abstract

A simple, accurate and reproducible reversed-phase high performance liquid chromatography method with fluorescence detection was developed for determination of octylphenol, nonylphenol and their short-chain ethoxylates, using an octadecyl silica column. The mobile phase used for the analysis consisted of methanol, acetonitrile and water (50:15:35). The analytes were separated successfully within a reasonable time without gradient elution, which was not achieved previously. Thus, use of inexpensive fluorescence detection instead of MS detection was enabled. This chromatographic method, combined with solid-phase extraction, was highly applicable for the simultaneous determination of octyl- and nonylphenol as well as their mono- and diethoxylates in real river water samples. The limit of detection (LOD) for octylphenol and its ethoxylates was 0.05 μg · L−1. For nonylphenol the LOD was 0.14 μg · L−1 and for its ethoxylates it was 0.15 μg · L−1. Recovery of octylphenol and its ethoxylates was about 80%. Recovery of nonylphenol and its ethoxylates was slightly lower (from 60 to 76%).

Kurzfassung

Eine einfache, genaue und reproduzierbare Umkehrphasen-Hochdruckflüssigkeitschromatographie mit Fluoreszenzdetektion wurde unter Verwendung einer Octadecyl-Silica-Säule für die Bestimmung von Octylphenol, Nonylphenol und ihrer kurzkettigen Ethoxylate entwickelt. Die für die Analyse verwendete mobile Phase bestand aus Methanol, Acetonitril und Wasser (50:15:35). Die Analyten wurden in einer angemessenen Zeit ohne Gradient-Elution erfolgreich getrennt, was bisher nicht erreicht wurde. Somit wurde eine kostengünstige Fluoreszenzdetektion anstatt einer MS Detektion ermöglicht. Diese Chromatographiemethode, kombiniert mit einer Festphasenextraktion, war in hohem Maße für die gleichzeitige Bestimmung von Octylphenol und Nonylphenol sowie für ihre Mono- and Diethoxylate in realen Flusswasserproben anwendbar. Die Nachweisgrenze (NWG) für Octylphenol und seiner Ethoxylate lag bei 0,05 μg · L−1 und für Nonylphenol und seiner Ethoxylate bei 0,15 μg · L−1. Die Wiederfindung von Octylphenol und seiner Ethoxylate lag bei ca. 80% und die von Nonylphenol und seiner Ethoxylate (von 60 bis 76%) etwas niedriger.


Agnieszka Zgoła-Grześkowiak, Poznan University of Technology, Institute of Chemistry and Technical Electrochemistry, ul. Piotrowo 3, 60-965 Poznań, Poland, Phone: +48616652033, Fax: +468616652571, E-Mail:

A. Zgoła-Grześkowiak graduated from the Poznan University of Technology in 1999 and she finished her PhD in 2003 there. Since then she has been working as Assistant Professor at the Poznan University of Technology.

T. Grześkowiak graduated from the Poznan University of Technology in 1995 and he finished his PhD in 2000 there. Since then he has been working outside the university as Quality Control Specialist. Nevertheless, he is realizing his interests working voluntarily at the Poznan University of Technology.


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Received: 2008-12-23
Revised: 2009-03-22
Published Online: 2013-04-02
Published in Print: 2009-07-01

© 2009, Carl Hanser Publisher, Munich

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