Skip to main page content
U.S. flag

An official website of the United States government

Dot gov

The .gov means it’s official.
Federal government websites often end in .gov or .mil. Before sharing sensitive information, make sure you’re on a federal government site.

Https

The site is secure.
The https:// ensures that you are connecting to the official website and that any information you provide is encrypted and transmitted securely.

Access keys NCBI Homepage MyNCBI Homepage Main Content Main Navigation
. 2023 Mar 1;71(8):3898-3905.
doi: 10.1021/acs.jafc.2c07873. Epub 2023 Feb 15.

Graphene-Type Materials for the Dispersive Solid-Phase Extraction Step in the QuEChERS Method for the Extraction of Brominated Flame Retardants from Capsicum Cultivars

Virgínia Cruz Fernandes  1 , Valentina F Domingues  1 , Marta S Nunes  2 , Renata Matos  2 , Iwona Kuźniarska-Biernacka  2 , Diana M Fernandes  2 , Antonio Guerrero-Ruiz  3 , Inmaculada Rodríguez Ramos  4 , Cristina Freire  2 , Cristina Delerue-Matos  1
Affiliations

Graphene-Type Materials for the Dispersive Solid-Phase Extraction Step in the QuEChERS Method for the Extraction of Brominated Flame Retardants from Capsicum Cultivars

Virgínia Cruz Fernandes et al. J Agric Food Chem. .

Abstract

A new application of graphene-type materials as an alternative cleanup sorbent in a quick, easy, cheap, effective, rugged, and safe (QuEChERS) procedure combined with GC-ECD/GC-MS/GC-MS/MS detection was successfully used for the simultaneous analysis of 12 brominated flame retardants in Capsicum cultivar samples. The chemical, structural, and morphological properties of the graphene-type materials were evaluated. The materials exhibited good adsorption capability of matrix interferents without compromising the extraction efficiency of target analytes when compared with other cleanups using commercial sorbents. Under optimal conditions, excellent recoveries were obtained, ranging from 90 to 108% with relative standard deviations of <14%. The developed method showed good linearity with a correlation coefficient above 0.9927, and the limits of quantification were in the range of 0.35-0.82 μg/kg. The developed QuEChERS procedure using reduced graphite oxide (rGO) combined with GC/MS was successfully applied in 20 samples, and the pentabromotoluene residues were quantified in two samples.

Keywords: Capsicum cultivars; QuEChERS; flame retardants; graphene-type material sorbents; peppers.

PubMed Disclaimer

Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
A—BFR mixture standard chromatogram at 50 μg/L. B—chromatograms obtained from an extract of C. annum L. spiked at 0.75 μg/kg using the CL3 (150 MgSO4 + 50 mg PSA + 50 mg C18 + 5 mg carbon) C—chromatograms obtained from an extract of C. annum L. spiked at 0.75 μg/kg using the CL7 (150 MgSO4 + 50 mg PSA +50 mg C18 + 5 mg S-GF) D—chromatograms obtained from an extract of C. annum L. spiked at 0.75 μg/kg using the CL5 (150 MgSO4 + 50 mg PSA + 50 mg C18 + 5 mg rGO).
Figure 2
Figure 2
Comparative recovery results between commercial d-SPE with commercial carbon (CL1) and graphene—dispersive sorbent materials (CL5 and CL7). Two-way ANOVA analysis with Sidak’s multiple comparison test (ns-non significant; ***-significant).
Figure 3
Figure 3
Recovery study comparing four cleanup sets with different amounts of commercial carbon (CL2 and CL3) and S-GF (CL6 and CL7). Two-way ANOVA analysis (ns-non significant; ****-significant)
Figure 4
Figure 4
Recovery study comparing four cleanup sets with different amounts of commercial carbon (CL2 and CL3) and rGO (CL4 and CL5). Two-way ANOVA analysis (ns-non significant; ****-significant).
See this image and copyright information in PMC

References

    1. Fernandes V. C.; Luts W.; Delerue-Matos C.; Domingues V. F. Improved QuEChERS for Analysis of Polybrominated Diphenyl Ethers and Novel Brominated Flame Retardants in Capsicum Cultivars Using Gas Chromatography. J. Agric. Food Chem. 2020, 68, 3260–3266. 10.1021/acs.jafc.9b07041. - DOI - PubMed
    1. Fernandes V. C.; Freitas M.; Pacheco J. G.; Fernandes Domingues V.; Delerue-Matos C. Evaluation of the QuEChERS and magnetic micro dispersive solid-phase extraction of brominated flame retardants in red fruits with determination by GC/MS. Food Chem. 2020, 309, 125572.10.1016/j.foodchem.2019.125572. - DOI - PubMed
    1. Dorosh O.; Fernandes V. C.; Moreira M. M.; Delerue-Matos C. Occurrence of pesticides and environmental contaminants in vineyards: Case study of Portuguese grapevine canes. Sci. Total Environ. 2021, 791, 148395.10.1016/j.scitotenv.2021.148395. - DOI - PubMed
    1. Hou R.; Lin L.; Li H.; Liu S.; Xu X.; Xu Y.; Jin X.; Yuan Y.; Wang Z. Occurrence, bioaccumulation, fate, and risk assessment of novel brominated flame retardants (NBFRs) in aquatic environments — A critical review. Water Res. 2021, 198, 117168.10.1016/j.watres.2021.117168. - DOI - PubMed
    1. Zacs D.; Perkons I.; Abdulajeva E.; Pasecnaja E.; Bartkiene E.; Bartkevics V. Polybrominated diphenyl ethers (PBDEs), hexabromocyclododecanes (HBCDD), dechlorane-related compounds (DRCs), and emerging brominated flame retardants (EBFRs) in foods: The levels, profiles, and dietary intake in Latvia. Sci. Total Environ. 2021, 752, 141996.10.1016/j.scitotenv.2020.141996. - DOI - PubMed