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How to confirm identified toxicants in effect-directed analysis

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Abstract

Due to the production and use of a multitude of chemicals in modern society, waters, sediments, soils and biota may be contaminated with numerous known and unknown chemicals that may cause adverse effects on ecosystems and human health. Effect-directed analysis (EDA), combining biotesting, fractionation and chemical analysis, helps to identify hazardous compounds in complex environmental mixtures. Confirmation of tentatively identified toxicants will help to avoid artefacts and to establish reliable cause–effect relationships. A tiered approach to confirmation is suggested in the present paper. The first tier focuses on the analytical confirmation of tentatively identified structures. If straightforward confirmation with neat standards for GC–MS or LC–MS is not available, it is suggested that a lines-of-evidence approach is used that combines spectral library information with computer-based structure generation and prediction of retention behaviour in different chromatographic systems using quantitative structure–retention relationships (QSRR). In the second tier, the identified toxicants need to be confirmed as being the cause of the measured effects. Candidate components of toxic fractions may be selected based, for example, on structural alerts. Quantitative effect confirmation is based on joint effect models. Joint effect prediction on the basis of full concentration–response plots and careful selection of the appropriate model are suggested as a means to improve confirmation quality. Confirmation according to the Toxicity Identification Evaluation (TIE) concept of the US EPA and novel tools of hazard identification help to confirm the relevance of identified compounds to populations and communities under realistic exposure conditions. Promising tools include bioavailability-directed extraction and dosing techniques, biomarker approaches and the concept of pollution-induced community tolerance (PICT).

Toxicity confirmation in EDA as a tiered approach

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Abbreviations

AhR:

arylhydrocarbon receptor

AMDIS:

Automated Mass Spectral Deconvolution and Identification System

BEQ:

benzo[a]pyrene equivalent quantity

BP:

boiling point

CA:

concentration addition

CALUX:

chemical-activated luciferase expression

ECX:

effect concentration required to achieve X% effect

EDA:

effect-directed analysis

EROD:

ethoxyresorufin-O-deethylase

DNA:

deoxyribonucleic acid

GC/MS:

gas chromatography with mass-selective detection

IA:

independent action

ICQ:

index of confirmation quality

IEQ:

induction equivalent quantities

IP:

identification points

LC-Q-TOF-MS:

liquid chromatography with a hybrid quadrupole–time-of-flight mass spectrometer

LSER:

linear solvation free-energy relationships

NIST:

National Institute of Standards and Technology

NMR:

nuclear magnetic resonance

PAH:

polycyclic aromatic hydrocarbon

PCB:

polychlorinated biphenyl

PCDD/F:

polychlorinated dibenzo-p-dioxin and furan

PDMS:

polydimethylsiloxane

PICT:

pollution-induced community tolerance

QSAR:

quantitative structure–activity relationship

QSRR:

quantitative structure–retention relationship

REP:

relative potency

RI:

retention index

RTL-W1:

rainbow trout liver cell line W1

SPMD:

semipermeable membrane device

TEQ:

toxicity equivalent quantity

TIE:

toxicity identification evaluation

TU:

toxic units

US EPA:

United States Environmental Protection Agency

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Acknowledgements

This study was funded by the European Union in the framework of the Integrated Project MODELKEY (Contract 511237-GOCE).

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Authors and Affiliations

  1. Department Effect-Directed Analysis, UFZ Helmholtz Centre for Environmental Research, Permoserstraße 15, 04318, Leipzig, Germany

    Werner Brack, Emma Schymanski, Georg Streck & Tobias Schulze

  2. Department Bioanalytical Ecotoxicology, UFZ Helmholtz Centre for Environmental Research, Permoserstraße 15, 04318, Leipzig, Germany

    Mechthild Schmitt-Jansen

  3. Veterinary Research Institute, Hudcova 70, 62132, Brno, Czech Republic

    Miroslav Machala

  4. Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, Barcelona, 08034, Spain

    Rikke Brix & Damià Barceló

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  1. Werner Brack
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Brack, W., Schmitt-Jansen, M., Machala, M. et al. How to confirm identified toxicants in effect-directed analysis. Anal Bioanal Chem 390, 1959–1973 (2008). https://doi.org/10.1007/s00216-007-1808-8

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