Identification of antimicrobial and glucocorticoid compounds in wastewater effluents with effect-directed analysis

Tim J.H. Jonkers; Corine J. Houtman; Yvonne van Oorschot; Marja H. Lamoree; Timo Hamers

doi:10.1016/j.envres.2023.116117

Identification of antimicrobial and glucocorticoid compounds in wastewater effluents with effect-directed analysis

Tim J.H. Jonkers, Corine J. Houtman, Yvonne van Oorschot, Marja H. Lamoree, Timo Hamers^*

^*Corresponding author for this work

Research output: Contribution to Journal › Article › Academic › peer-review

Abstract

Pharmaceuticals, such as glucocorticoids and antibiotics, are inadequately removed from wastewater and may cause unwanted toxic effects in the receiving environment. This study aimed to identify contaminants of emerging concern in wastewater effluent with antimicrobial or glucocorticoid activity by applying effect-directed analysis (EDA). Effluent samples from six wastewater treatment plants (WWTPs) in the Netherlands were collected and analyzed with unfractionated and fractionated bioassay testing. Per sample, 80 fractions were collected and in parallel high-resolution mass spectrometry (HRMS) data were recorded for suspect and nontarget screening. The antimicrobial activity of the effluents was determined with an antibiotics assay and ranged from 298 to 711 ng azithromycin equivalents·L⁻¹. Macrolide antibiotics were identified in each effluent and found to significantly contribute to the antimicrobial activity of each sample. Agonistic glucocorticoid activity determined with the GR-CALUX assay ranged from 98.1 to 286 ng dexamethasone equivalents·L⁻¹. Bioassay testing of several tentatively identified compounds to confirm their activity revealed inactivity in the assay or the incorrect identification of a feature. Effluent concentrations of glucocorticoid active compounds were estimated from the fractionated GR-CALUX bioassay response. Subsequently, the biological and chemical detection limits were compared and a sensitivity gap between the two monitoring approaches was identified. Overall, these results emphasize that combining sensitive effect-based testing with chemical analysis can more accurately reflect environmental exposure and risk than chemical analysis alone.

Original language	English
Article number	116117
Pages (from-to)	1-9
Number of pages	9
Journal	Environmental Research
Volume	231
Early online date	12 May 2023
DOIs	https://doi.org/10.1016/j.envres.2023.116117
Publication status	Published - 15 Aug 2023

Bibliographical note

Funding Information:
The authors gratefully acknowledge Joop Baltussen for providing access to the samples of the EPRTR monitoring campaign. BioDetection systems B.V. is acknowledged for providing the GR-CALUX cell line. This work is part of the research program RoutinEDA with project number 15747, which is (partly) financed by the Dutch Research Council (NWO).

Publisher Copyright:
© 2023 The Authors

Funding

The authors gratefully acknowledge Joop Baltussen for providing access to the samples of the EPRTR monitoring campaign. BioDetection systems B.V. is acknowledged for providing the GR-CALUX cell line. This work is part of the research program RoutinEDA with project number 15747, which is (partly) financed by the Dutch Research Council (NWO).

Funders	Funder number
Not added	195.068.662

Keywords

Antibiotic
Bioassay
Effect-directed analysis
Glucocorticoid
Suspect and nontarget screening
Wastewater

UN SDGs

This output contributes to the following UN Sustainable Development Goals (SDGs)

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10.1016/j.envres.2023.116117

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Cite this

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title = "Identification of antimicrobial and glucocorticoid compounds in wastewater effluents with effect-directed analysis",

abstract = "Pharmaceuticals, such as glucocorticoids and antibiotics, are inadequately removed from wastewater and may cause unwanted toxic effects in the receiving environment. This study aimed to identify contaminants of emerging concern in wastewater effluent with antimicrobial or glucocorticoid activity by applying effect-directed analysis (EDA). Effluent samples from six wastewater treatment plants (WWTPs) in the Netherlands were collected and analyzed with unfractionated and fractionated bioassay testing. Per sample, 80 fractions were collected and in parallel high-resolution mass spectrometry (HRMS) data were recorded for suspect and nontarget screening. The antimicrobial activity of the effluents was determined with an antibiotics assay and ranged from 298 to 711 ng azithromycin equivalents·L−1. Macrolide antibiotics were identified in each effluent and found to significantly contribute to the antimicrobial activity of each sample. Agonistic glucocorticoid activity determined with the GR-CALUX assay ranged from 98.1 to 286 ng dexamethasone equivalents·L−1. Bioassay testing of several tentatively identified compounds to confirm their activity revealed inactivity in the assay or the incorrect identification of a feature. Effluent concentrations of glucocorticoid active compounds were estimated from the fractionated GR-CALUX bioassay response. Subsequently, the biological and chemical detection limits were compared and a sensitivity gap between the two monitoring approaches was identified. Overall, these results emphasize that combining sensitive effect-based testing with chemical analysis can more accurately reflect environmental exposure and risk than chemical analysis alone.",

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note = "Funding Information: The authors gratefully acknowledge Joop Baltussen for providing access to the samples of the EPRTR monitoring campaign. BioDetection systems B.V. is acknowledged for providing the GR-CALUX cell line. This work is part of the research program RoutinEDA with project number 15747, which is (partly) financed by the Dutch Research Council (NWO). Publisher Copyright: {\textcopyright} 2023 The Authors",

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doi = "10.1016/j.envres.2023.116117",

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AU - Lamoree, Marja H.

AU - Hamers, Timo

N1 - Funding Information: The authors gratefully acknowledge Joop Baltussen for providing access to the samples of the EPRTR monitoring campaign. BioDetection systems B.V. is acknowledged for providing the GR-CALUX cell line. This work is part of the research program RoutinEDA with project number 15747, which is (partly) financed by the Dutch Research Council (NWO). Publisher Copyright: © 2023 The Authors

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N2 - Pharmaceuticals, such as glucocorticoids and antibiotics, are inadequately removed from wastewater and may cause unwanted toxic effects in the receiving environment. This study aimed to identify contaminants of emerging concern in wastewater effluent with antimicrobial or glucocorticoid activity by applying effect-directed analysis (EDA). Effluent samples from six wastewater treatment plants (WWTPs) in the Netherlands were collected and analyzed with unfractionated and fractionated bioassay testing. Per sample, 80 fractions were collected and in parallel high-resolution mass spectrometry (HRMS) data were recorded for suspect and nontarget screening. The antimicrobial activity of the effluents was determined with an antibiotics assay and ranged from 298 to 711 ng azithromycin equivalents·L−1. Macrolide antibiotics were identified in each effluent and found to significantly contribute to the antimicrobial activity of each sample. Agonistic glucocorticoid activity determined with the GR-CALUX assay ranged from 98.1 to 286 ng dexamethasone equivalents·L−1. Bioassay testing of several tentatively identified compounds to confirm their activity revealed inactivity in the assay or the incorrect identification of a feature. Effluent concentrations of glucocorticoid active compounds were estimated from the fractionated GR-CALUX bioassay response. Subsequently, the biological and chemical detection limits were compared and a sensitivity gap between the two monitoring approaches was identified. Overall, these results emphasize that combining sensitive effect-based testing with chemical analysis can more accurately reflect environmental exposure and risk than chemical analysis alone.

AB - Pharmaceuticals, such as glucocorticoids and antibiotics, are inadequately removed from wastewater and may cause unwanted toxic effects in the receiving environment. This study aimed to identify contaminants of emerging concern in wastewater effluent with antimicrobial or glucocorticoid activity by applying effect-directed analysis (EDA). Effluent samples from six wastewater treatment plants (WWTPs) in the Netherlands were collected and analyzed with unfractionated and fractionated bioassay testing. Per sample, 80 fractions were collected and in parallel high-resolution mass spectrometry (HRMS) data were recorded for suspect and nontarget screening. The antimicrobial activity of the effluents was determined with an antibiotics assay and ranged from 298 to 711 ng azithromycin equivalents·L−1. Macrolide antibiotics were identified in each effluent and found to significantly contribute to the antimicrobial activity of each sample. Agonistic glucocorticoid activity determined with the GR-CALUX assay ranged from 98.1 to 286 ng dexamethasone equivalents·L−1. Bioassay testing of several tentatively identified compounds to confirm their activity revealed inactivity in the assay or the incorrect identification of a feature. Effluent concentrations of glucocorticoid active compounds were estimated from the fractionated GR-CALUX bioassay response. Subsequently, the biological and chemical detection limits were compared and a sensitivity gap between the two monitoring approaches was identified. Overall, these results emphasize that combining sensitive effect-based testing with chemical analysis can more accurately reflect environmental exposure and risk than chemical analysis alone.

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KW - Glucocorticoid

KW - Suspect and nontarget screening

KW - Wastewater

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JF - Environmental Research

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ER -

Identification of antimicrobial and glucocorticoid compounds in wastewater effluents with effect-directed analysis

Abstract

Bibliographical note

Funding

Keywords

UN SDGs

Access to Document

Persistent URL (handle)

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