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  • Determination of alkylphenols and 17beta-estradiol in fish homogenate. Extraction and clean-up strategies.

Determination of alkylphenols and 17beta-estradiol in fish homogenate. Extraction and clean-up strategies.

Journal of chromatography. A (2010-08-17)
P Navarro, J Bustamante, A Vallejo, A Prieto, A Usobiaga, S Arrasate, E Anakabe, E Puy-Azurmendi, O Zuloaga
ABSTRACT

The determination of target analytes such as nonyl- and octylphenols and 17beta-estradiol in fish homogenate require of solid-liquid extraction step. In this work microwave-assisted extraction (MAE) and focused-ultrasound liquid extraction (FUSLE) were studied as two different alternatives for extraction of the target compounds in zebrafish (Danio rerio) homogenate. In this work solid phase extraction (SPE) using 5-g and 10-g Florisil cartridges and gel permeation chromatography (GPC) were studied for the clean-up of the MAE and FUSLE extracts due to the non-selective extraction step. Although good recoveries were obtained both for SPE (106% and 126% range) and GPC (79% and 100% range) clean-up procedures, cleaner chromatograms were obtained after SPE and finally 5-g Florisil cartridges were tested since no improvement was observed when 10-g Florisil cartridges were used. Under optimized clean-up conditions, MAE and FUSLE provided comparable results for 4nOP and NP, while more accurate results were obtained for 4tOP and E2 after FUSLE. Finally, the method was applied to the determination of alkylphenols and 17beta-estradiol in zebrafish homogenate that had been exposed to known concentrations of the target analytes. In the case of alkylphenols two different isomers of nonyl- and octylphenol (4-(3',6'-dimethyl-3'-hepthyl)phenol, 363-NP, and 4-(3'-methyl-3'-hepthyl)phenol, 33-OP) were studied.

MATERIALS
Product Number
Brand
Product Description

Supelco
Florisil® Adsorbent for Chromatography, 30-60 mesh
Supelco
Florisil® Adsorbent for Chromatography, 60-100 mesh
Sigma-Aldrich
Florisil®, 100-200 mesh
Supelco
Florisil®, PR grade, 60-100 mesh, coarse powder
Supelco
Florisil®, 100-200 mesh, fine powder
Supelco
Florisil®, for the determination of hydrocarbon acc. to ISO 9377-2
Supelco
Florisil®, <200 mesh, fine powder
Supelco
Florisil® PR, PR grade (analysis acc. to FDA)