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Determination of perfluorinated compounds in aquatic organisms: a review

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Abstract

Bioaccumulation of PFAS in aquatic organisms is an environmental problem of growing concern around the world. This problem has been tackled by regulatory bodies by proposing EQS for biota in EU water bodies and tolerable daily intake for food. The introduction of regulatory limits requires the availability of harmonised and validated analytical methods of sufficient sensitivity. This paper reviews recent advances in analytical methods for analysis of PFAS in aquatic organisms. The methods available for biota analysis are mostly based on three extraction procedures: ion-pair extraction, solvent liquid extraction, and alkaline digestion. The resulting extracts are then subjected to different clean-up or enrichment steps on solid adsorbents, for example graphitized carbon black, C18, and WAX phases. All methods reviewed in this work give reliable results but are partially validated only, because of the lack of certified reference materials and regular interlaboratory exercises. The few interlaboratory exercises performed on real unspiked samples did not afford satisfactory results for PFAS other than PFOS, especially for matrices with high lipid content, for example mussels. The reasons for those partially negative results have been identified, and can mainly be attributed to calibration procedures and availability and purity of standards. The urgent need for certified reference materials for this type of analysis is emphasized.

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Abbreviations

6–2 FTUCA:

2H-Perfluoro-2-octenoic acid

7–1 FTOH:

Pentadecafluoro-1-octanol

7–3 FTCA:

2H,2H,3H,3H-Pentadecafluorodecanoic acid

7–3 FTUCA:

2H,3H-Pentadecafluoro-2-decenoic acid

8–2 FTCA:

2H,2H-Heptadecafluorodecanoic acid

8–2 FTUCA:

2H-Hexadecafluoro-2-decenoic acid

10–1 FTOH:

1H,1H-Perfluoro-1-undecanol

10–2 FTCA:

2H,2H-Nonadecafluorododecanoic acid

10–2 FTUCA:

2H-Octadecafluoro-2-dodecenoic acid

7H-PFHpA:

7H-Perfluoroheptanoic acid

BPTA:

3,5-Bis(trifluoromethyl)phenylacetic acid

CRM:

Certified reference material

dw:

Dry weight

EPI:

Enhanced product ion

EQS:

Environmental quality standard

ESI:

Electrospray ionization

FTCA:

Fluorotelomer carboxylate

FTOH:

Fluorotelomer alcohols

FTUCA:

Fluorotelomer unsaturated carboxylate

GC-PCI-MS:

Gas chromatography–positive chemical ionization mass spectrometry

IDA:

Information-dependent acquisition mode

i,p-PFNA:

Perfluoro-7-methyloctanoic acid

IPE:

Ion-pair extraction

IS:

Internal standard

IT:

Ion trap

LOD:

Limit of detection

LOQ:

Limit of quantification

MSPD:

Matrix solid-phase dispersion

MTBE:

Methyl tert-butyl ether

N-ethyl FOSA:

N-Ethylperfluorooctanesulfonamide

N-ethyl FOSE:

N-Ethylperfluorooctanesulfonamidoethanol

N-ethyl PFOSA:

N-Ethylperfluorooctanesulfonamide

N-methyl FOSA:

N-Methylperfluorooctanesulfonamide

N-methyl FOSE:

N-Methylperfluorooctanesulfonamidoethanol

N,N-diethyl PFOSA:

N,N-Diethylperfluorooctanesulfonamide

PFAS:

Perfluoroalkyl substances

PFBA:

Perfluorobutanoic acid

PFBS:

Perfluorobutanesulfonate

PFCA:

Perfluorocarboxylic acids

PFDA:

Perfluorodecanoic acid

PFDoDA:

Perfluorododecanoic acid

PFDPA:

Perfluorodecylphosphonic acid

PFDS:

Perfluorodecanesulfonate

PFHxA:

Perfluorohexanoic acid

PFHxDA:

Perfluorohexadecanoic acid

PFHxPA:

Perfluorohexylphosphonic acid

PFHxS:

Perfluorohexanesulfonic acid

PFHpA:

Perfluoroheptanoic acid

PFNA:

Perfluorononanoic acid

PFOA:

Perfluorooctanoic acid

PFOcDA:

Perfluorooctadecanoic acid

PFOPA:

Perfluorooctylphosphonic acid

PFOS:

Perfluorooctanesulfonic acid

PFOSA:

Perfluorooctanesulfonamide

PFOSi:

Pefluorooctanesulfinate

PFPA:

Perfluorinated phosphonic acids

PFPeA:

Perfluoropentanoic acid

PFSA:

Perfluorosulfonic acids

PFTeDA:

Perfluorotetradecanoic acid

PFUnDA:

Perfluoroundecanoic acid

PLE:

Pressurized liquid extraction

QqLIT:

Triple-quadrupole with linear trap

QqQ:

Triple quadrupole

QTOF:

Quadrupole time-of-flight

QuEChERS:

Quick easy, cheap, rugged and safe

RSD:

Relative standard deviation

SLE:

Solid–liquid extraction

SPE:

Solid phase extraction

SRM:

Selected reaction monitoring

TBA:

Tetrabutylammonium hydrogen sulfate

THF:

Tetrahydrofuran

THPFOS:

1H,1H,2H,2H-Perfluorooctanesulfonic acid

TOF:

Time-of-flight

UE:

Ultrasonic extraction

WAX:

Weak anion exchange

ww:

Wet weight

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Acknowledgments

The authors acknowledge the fundamental contribution of anonymous referees to improvement of this paper. They also warmly thank Claudia Martins (Thermo Fisher) for her valuable comments and suggestions during the revision process.

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Authors and Affiliations

  1. CNR-IRSA, Water Research Institute, Via del Mulino 19, 20861, Brugherio, MB, Italy

    Sara Valsecchi, Marianna Rusconi & Stefano Polesello

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  1. Sara Valsecchi
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  2. Marianna Rusconi
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  3. Stefano Polesello
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Correspondence to Stefano Polesello.

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Published in the topical collection Emerging Contaminants in Biota with guest editors Yolanda Picó and Damià Barceló.

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Valsecchi, S., Rusconi, M. & Polesello, S. Determination of perfluorinated compounds in aquatic organisms: a review. Anal Bioanal Chem 405, 143–157 (2013). https://doi.org/10.1007/s00216-012-6492-7

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