Food Analytical Methods

, Volume 11, Issue 9, pp 2485–2496 | Cite as

Rapid Sample Preparation Method with High Lipid Removal Efficiency for Determination of Sulphuric Acid Stable Organic Compounds in Fish Samples

  • P. Tölgyessy
  • S. Nagyová


A rapid and low-cost sample preparation method modifying the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method was developed for the determination of H2SO4 stable organic compounds in fish samples. The method involves acetonitrile salting-out extraction and a novel clean-up procedure combining the pH-tuned dispersive liquid–liquid microextraction (DLLME) with conc. H2SO4 digestion. The H2SO4 treatment is carried out by a simple operation in contrast to laborious and time-consuming procedures reported in the literature. The method was developed, optimised and validated using selected polybrominated diphenyl ethers (PBDEs) as representatives of H2SO4 stable compounds. For instrumental analysis of sample extracts, thermal desorption–gas chromatography–triple quadrupole tandem mass spectrometry (TD–GC–QqQ-MS/MS) was used. The proposed sample preparation method provides better co-extractives removal efficiency as compared to the original QuEChERS method and, unlike the QuEChERS dispersive solid-phase extraction (dSPE), allows complete removal of fatty acids. The sample preparation is low-cost due to the employment of small amounts of low-cost chemicals (no need of expensive sorbents), and it does not require special instrumentation. The whole analytical method showed satisfactory performance (linearity, recovery, repeatability, accuracy, limits of the method), and its applicability was confirmed by determination of PBDEs in samples of four fish species with variable lipid content in the range of 0.7–19%. The obtained recoveries for six PBDEs in the NIST standard reference material SRM 1946 were in the range of 81–95%, and relative standard deviations were in the range of 3–13%.


Sample preparation QuEChERS Dispersive liquid–liquid microextraction Sulphuric acid treatment Fish samples 



Financial support from the EU Cohesion Funds within the project Monitoring and Assessment of Water Body Status (No. 310011A366 Phase III) is acknowledged.

Compliance with Ethical Standards

Conflict of Interest

P. Tölgyessy declares that he has no conflict of interest. S. Nagyová declares that he has no conflict of interest.

Ethical Approval

All applicable international, national and institutional guidelines for the care and use of animals were followed.

Informed Consent

Not applicable.


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© Springer Science+Business Media, LLC, part of Springer Nature 2018

Authors and Affiliations

  1. 1.Slovak National Water Reference LaboratoryWater Research InstituteBratislavaSlovak Republic

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