Reversed-Phase Dispersive Liquid-Liquid Microextraction (RP-DLLME) as a Green Sample Preparation Method for Multielement Determination in Fish Oil by ICP-OES
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A new and simple method for Cd, Fe, Mn, Ni, Pb, and Zn determination in fish oil by inductively coupled plasma optical emission spectrometry (ICP-OES) was developed using reversed-phase dispersive liquid-liquid microextraction (RP-DLLME) for sample preparation. The RP-DLLME method was based on the simultaneous extraction and pre-concentration of analytes in fish oil, using 10.0 g of sample preheated (75 °C), with the addition of a dispersant/extractant mixture (n-propanol/diluted HNO3 solution). After stirring and centrifugation (5600g, 10 min), the aqueous phase was used for analyte determination. The RP-DLLME method was performed using only 700 μL of n-propanol and 300 μL of 2.0 mol L−1 HNO3 solution. The recoveries for Cd, Mn, Ni, and Zn using the spikes of 100 and 500 μg kg−1 ranged from 86.4 to 93.4% and 90.4 to 97.3%, respectively. For Fe and Pb, the recoveries ranged from 85.7 and 90.0% and 85.3 and 94.4% for the same spikes. The limits of quantification (LOQs) were 0.41, 1.98, 0.33, 0.35, 1.52, and 1.39 μg kg−1 for Cd, Fe, Mn, Ni, Pb, and Zn, respectively. The proposed RP-DLLME sample preparation method allowed analyte extraction for further determination by ICP-OES using a small amount of diluted HNO3 solution avoiding applying a sample decomposition step. The extract was suitable for direct introduction in the ICP-OES equipment and reached LOQs values lower than similar methods from literature. Finally, the proposed analytical method was viable and this is the first application of RP-DLLME for animal source fat combined with ICP-OES determination.
KeywordsInductively coupled plasma optical emission spectrometry Microextraction Omega 3 Pre-concentration Recovery test Sample preparation
This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - Brasil (CAPES) - Finance Code 001.
Compliance with Ethical Standards
Conflict of Interest
Daneysa Lahis Kalschne declares that she has no conflict of interest. Cristiane Canan declares that she has no conflict of interest. Juliano Smanioto Barin declares that he has no conflict of interest. Rochele Sogari Picoloto declares that she has no conflict of interest. Oldair Donizete Leite declares that he has no conflict of interest. Éder Lisandro de Moraes Flores declares that he has no conflict of interest.
This article does not contain any studies with human participants or animals performed by any of the authors.
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