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. 2022 Jan 1;10(1):12.
doi: 10.3390/toxics10010012.

Critical Assessment of Clean-Up Techniques Employed in Simultaneous Analysis of Persistent Organic Pollutants and Polycyclic Aromatic Hydrocarbons in Fatty Samples

Lucie Drábová  1 , Darina Dvořáková  1 , Kateřina Urbancová  1 , Tomáš Gramblička  1 , Jana Hajšlová  1 , Jana Pulkrabová  1
Affiliations

Critical Assessment of Clean-Up Techniques Employed in Simultaneous Analysis of Persistent Organic Pollutants and Polycyclic Aromatic Hydrocarbons in Fatty Samples

Lucie Drábová et al. Toxics. .

Abstract

Interference of residual lipids is a very common problem in ultratrace analysis of contaminants in fatty matrices. Therefore, quick and effective clean-up techniques applicable to multiple groups of analytes are much needed. Cartridge and dispersive solid-phase extraction (SPE and dSPE) are often used for this purpose. In this context, we evaluated the lipid clean-up efficiency and performance of four commonly used sorbents-silica, C18, Z-Sep, and EMR-lipid-for the determination of organic pollutants in fatty fish samples (10%) extracted using ethyl acetate or the QuEChERS method. Namely, 17 polychlorinated biphenyls (PCBs), 22 organochlorine pesticides (OCPs), 13 brominated flame retardants (BFRs), 19 per- and polyfluoroalkyl substances (PFAS), and 16 polycyclic aromatic hydrocarbons (PAHs) were determined in this study. The clean-up efficiency was evaluated by direct analysis in real time coupled with time-of-flight mass spectrometry (DART-HRMS). The triacylglycerols (TAGs) content in the purified extracts were significantly reduced. The EMR-lipid sorbent was the most efficient of the dSPE sorbents used for the determination of POPs and PAHs in this study. The recoveries of the POPs and PAHs obtained by the validated QuEChERS method followed by the dSPE EMR-lipid sorbent ranged between 59 and 120%, with repeatabilities ranging between 2 and 23% and LOQs ranging between 0.02 and 1.50 µg·kg-1.

Keywords: EMR-lipid; GC-MS/MS; LC-MS/MS; PAHs; POPs; clean-up; fish.

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Conflict of interest statement

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

Figures

Figure 1
Figure 1
Flow charts of the tested methods.
Figure 2
Figure 2
The amount of matrix co-extracts determined gravimetrically in smoked trout extracts before and after purification employing various sorbents for SPE and dSPE. Error bars display the repeatability of the procedure.
Figure 3
Figure 3
The comparison of TAG removal (scanned mass range m/z 800–1000) between the crude and purified extracts of the smoked trout using different sorbents detected by DART-HRMS.
Figure 4
Figure 4
An example of the GC-MS/MS chromatogram in multi reaction monitoring (MRM) mode of a smoked trout sample spiked with PAHs. MeCN extract purified using (2) silica SPE minicolumn and (5) dSPE EMR-lipid. MRM transitions shown: CPP-226 > 226; BaA, CHR-228 > 228, BbFA, BkFA, BjFA, BaP-252 > 252.
Figure 5
Figure 5
Matrix effects using the tested sorbents (C18, Z-Sep and EMR-lipid) on LC-MS/MS. Response 100% = no matrix effect; response < 100% = signal suppression (e.g., response 40% corresponds to 60% suppression of signal by matrix effects); and response > 100% = signal enhancement.
See this image and copyright information in PMC

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