Reversed-Phase Dispersive Liquid-Liquid Microextraction (RP-DLLME) as a Green Sample Preparation Method for Multielement
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Reversed-Phase Dispersive Liquid-Liquid Microextraction (RP-DLLME) as a Green Sample Preparation Method for Multielement Determination in Fish Oil by ICP-OES Daneysa Lahis Kalschne 1 & Cristiane Canan 1 & Juliano Smanioto Barin 2 & Rochele Sogari Picoloto 3 & Oldair Donizete Leite 4 & Eder Lisandro Moraes Flores 4 Received: 4 April 2019 / Accepted: 15 July 2019 # Springer Science+Business Media, LLC, part of Springer Nature 2019
Abstract 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 RPDLLME 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. Keywords Inductively coupled plasma optical emission spectrometry . Microextraction . Omega 3 . Pre-concentration . Recovery test . Sample preparation
Introduction Fish oil is an important source of omega-3 polyunsaturated fatty acids, which is available commercially in capsules used for diet supplementation. EPA (cis-5, 8,11,14,17 * Eder Lisandro Moraes Flores [email protected] Daneysa Lahis Kalschne [email protected]
eicosapentaenoic acid) and DHA (cis-4, 7, 10,13,16,19 docosahexaenoic acid) are essential fatty acids found in fish oil and may play a beneficial role in several human pathologies, such as obesity and diabetes mellitus type 2, are also associated with a reduced incidence of stroke and 1
Departamento de Alimentos, Universidade Tecnológica Federal do Paraná, Avenida Brasil, 4232, Bairro Independência, Medianeira, PR 85884-000, Brazil
2
Departamento de Tecnologia e Ciência dos Alimentos, Universidade Federal de Santa Maria, Av. Roraima, 1000, Cidade Universitária, Camobi, Santa Maria, RS 97105-900, Brazil
3
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