Progress of Cryogenics and Isotopes Separation , ISSN: 1582-2575
2019, Volume 22, Issue 2
Pages 43-54

Assessment of PAHs levels in sediments and fish collected from artificial lakes on the course of Olt river, Romania: Optimisation and validation of the extraction methods

Corina Teodora Ciucure , Elisabeta-Irina Geana *

National Research and Development Institute for Cryogenics and Isotopic Technologies - ICSI Rm. Valcea, Uzinei Street no. 4, PO Box Râureni 7, 240050, Râmnicu Vâlcea, Romania

*Corresponding author: Elisabeta-Irina Geana, E mail: irina.geana@icsi.ro

Received 20 September 2019Received in revised form 15 October 2019Accepted 17 October 2019Available online 20 November 2019


Abstract

In this work the procedures for the analysis of 15 prioritary PAHs in sediment and fish samples were optimised and validated. Different extraction protocoles: Energized Dispersive Extraction (EDGE) and ultrasonic solvent extraction procedures with hexane:acetone 1:1 and dichloromethane for sediments and solid-lichid extraction procedure combined with lipids hydrolysis with potassium hydroxide for fish, were used for PAHs isolation from sediments and fish material prior to HPLC-FL analysis. General analytical procedures were validated by systematic recovery experiments using sediment standard reference material ERM-CC013a and by spiking experiments at three levels in the case of fish.
The targeted priority PAHs, except naphthalene, acenaphthene and dibenz(a,h)anthracene, were successfully extracted from ERM-CC013a certified material, with recoveries ranging from 61.9-125.2 % with variation coefficients not exceeding 10%. Ultrasonic extraction procedure with dichloromethane during 30 min presented good analytical performances (recoveries ranging from 79.0% to 103.3%, precision within 10% for all the PAHs, quantification limits ranging from 0.05-0.94 μg/kg). In the case of fish matrix, the extraction procedure shows satisfactory recoveries, facilitating the determination of all PAHs regulated well below the value of the concentrations imposed today. Limits of quantification (LOQs) ranged between 0.065-0.675 μg/kg fresh fish.
The optimised procedures were applied to assess the level of 15 PAHs in the sediments and fish samples from artificial lackes on the middle and lower course of Olt river, Romania, during January and February 2019, in order to estimate the concentrations and possible origins of contamination and to assess the safety concerning PAHs contents of different fish species.


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  • Keywords

    PAHs, sediments, fish, extraction methods, validation


    Tag search PAHs sediments fish extraction methods validation