Food Analytical Methods

, Volume 13, Issue 1, pp 230–237 | Cite as

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
  • Cristiane Canan
  • Juliano Smanioto Barin
  • Rochele Sogari Picoloto
  • Oldair Donizete Leite
  • Eder Lisandro Moraes FloresEmail author


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.


Inductively coupled plasma optical emission spectrometry Microextraction Omega 3 Pre-concentration Recovery test Sample preparation 


Funding Information

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.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.


  1. Bakircioglu D, Topraksever N, Kurtulus YB (2015) Separation/preconcentration system based on emulsion-induced breaking procedure for determination of cadmium in edible oil samples by flow injection-flame atomic absorption spectrometry. Food Anal Methods 8:2178–2184CrossRefGoogle Scholar
  2. Brasil (2013) Resolução RDC n° 42 de 29 de Agosto de 2013 (RDC 42-2013). Accessed 20 July 2019
  3. Cabrera-Vique C, Bouzas PR, Oliveras-López MJ (2012) Determination of trace elements in extra virgin olive oils: a pilot study on the geographical characterisation. Food Chem 134:434–439CrossRefGoogle Scholar
  4. Chaves ES, Loos-Vollebregt MTC, Curtius AJ, Vanhaecke F (2011) Determination of trace elements in biodiesel and vegetable oil by inductively coupled plasma optical emission spectrometry following alcohol dilution. Spectrochim Acta B At Spectrosc 66:733–739CrossRefGoogle Scholar
  5. Codex Alimentarius (1995) Codex general standard for contaminants and toxins in food and fees (CODEX STAN 193-1995). Accessed 20 July 2019
  6. Codex Alimentarius (1999) Codex standard for named vegetable oils (CODEX-STAN 210-1999). Accessed 20 July 2019
  7. Corazza MZ, Tarley CRT (2016) Development and feasibility of emulsion breaking method for the extraction of cadmium from omega-3 dietary supplements and determination by flow injection TS-FF-AAS. Microchem J 127:145–151CrossRefGoogle Scholar
  8. Ennoukh FE, Bchitou R, Mohammed F, Guillaume D, Harhar H, Bouhaouss A (2017) Study of the effects of extraction methods on argan oil quality through its metal content. Ind Crop Prod 109:182–184CrossRefGoogle Scholar
  9. European Comittee (2006) Setting maximum levels for certain contaminants in foofstuffs (EC 1881-2006). Accessed 20 July 2019Google Scholar
  10. González AG, Herrador MA (2007) A practical guide to analytical method validation, including measurement uncertainty and accuracy profiles. TrAC Trends Anal Chem 26:227–238CrossRefGoogle Scholar
  11. López-García I, Vicente-Martínez Y, Hernández-Córdoba M (2014) Determination of cadmium and lead in edible oils by electrothermal atomic absorption spectrometry after reverse dispersive liquid-liquid microextraction. Talanta 124:106–110CrossRefGoogle Scholar
  12. Lourenço EC, Eyng E, Bittencourt PRS, Duarte FA, Picoloto RS, Flores ÉLM (2019) A simple, rapid and low cost reversed-phase dispersive liquid-liquid microextraction for the determination of Na, K, Ca and Mg in biodiesel. Talanta 199:1–7CrossRefGoogle Scholar
  13. Mitić M, Pavlović A, Tošić S, Mašković P, Kostić D, Mitić S, Kocić C, Mašković J (2018) Optimization of simultaneous determination of metals in commercial pumpkin seed oils using inductively coupled atomic emission spectrometry. Microchem J 141:197–203CrossRefGoogle Scholar
  14. Mohammed F, Abdulwali N, Guillaume D, Tenyang N, Ponka R, Al-Gadabi K, Bchitoub R, Abdullahg AH, Najih KM (2018) Chemical composition and mineralogical residence of sesame oil from plants grown in different Yemeni environments. Microchem J 140:269–277CrossRefGoogle Scholar
  15. Rezaee M, Assadi Y, Milani Hosseini MR, Aghaee E, Ahmadi F, Berijani S (2006) Determination of organic compounds in water using dispersive liquid-liquid microextraction. J Chromatogr A 1116:1–9CrossRefGoogle Scholar
  16. Rosa FC, Duarte FA, Paniz JNG, Heidrich GM, Nunes MAG, Flores EMM, Dressler VL (2015) Dispersive liquid-liquid microextraction: an efficient approach for extraction of Cd and Pb from honey and determination by flame atomic absorption spectrometry. Microchem J 123:211–217CrossRefGoogle Scholar
  17. Schneider M, Pereira ÉR, Quadros DPC, Welz B, Carasek E, Andrade JB, Menoyo JC, Feldmann J (2017) Investigation of chemical modifiers for the determination of cadmium and chromium in fish oil and lipoid matrices using HR-CS GF AAS and a simple ‘dilute-and-shoot’ approach. Microchem J 133:175–181CrossRefGoogle Scholar
  18. Seeger TS, Vecchia PD, Machado EQ, Reinke K, Mesko MF, Duarte FA (2017) Feasibility of DLLME for the extraction and preconcentration of As and Cd in sugar for further determination by ICP-MS. J Braz Chem Soc 28:1691–1697Google Scholar
  19. Sokoła-Wysoczanska E, Wysoczanski T, Wagner J, Czyz K, Bodkowski R, Lochynski S, Patkowska-Sokoła B (2018) Polyunsaturated fatty acids and their potential therapeutic role in cardiovascular system disorders - a review. Nutrients 10:1–21CrossRefGoogle Scholar
  20. Todolí JL, Mermet JM (1999) Acid interferences in atomic spectrometry: analyte signal effects and subsequent reduction. Spectrochim Acta B At Spectrosc 54:895–929CrossRefGoogle Scholar
  21. Trindade ASN, Dantas AF, Lima DC, Ferreira SLC, Teixeira LSG (2015) Multivariate optimization of ultrasound-assisted extraction for determination of Cu, Fe, Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry. Food Chem 185:145–150CrossRefGoogle Scholar

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© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Departamento de AlimentosUniversidade Tecnológica Federal do ParanáMedianeiraBrazil
  2. 2.Departamento de Tecnologia e Ciência dos AlimentosUniversidade Federal de Santa MariaSanta MariaBrazil
  3. 3.Departamento de QuímicaUniversidade Federal de Santa MariaSanta MariaBrazil
  4. 4.Departamento de QuímicaUniversidade Tecnológica Federal do ParanáMedianeiraBrazil

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