Effect-directed analysis and suspect screening to identify potential toxic drivers in water

Sofia Lindblad

doi:10.54612/a.5uaek3dad6

Effect-directed analysis and suspect screening to identify potential toxic drivers in water

Bidragets översatta titel: Effektdriven analys och suspect screening för att identifiera potentiellt toxicitetdrivande ämnen i vatten

Sofia Lindblad

Institutionen för vatten och miljö

Publikation: Avhandling › Doktorsavhandling

6 Nedladdningar

Sammanfattning

En metod för effektdriven analys (EDA), baserad på den nya tekniken högkapacitetsfraktionering, ultra-högtrycks vätskekromatografi högupplöst masspektrometri (UPLC-HRMS), och ett bioanalysbatteri riktat mot fyra olika biologiska targets utvecklades. Bioanalyserna använde sig av östrogenreceptor (ER), androgen receptor (AR), arylkolvätereceptor (AR) och nukleär faktor erytroid 2- relaterad faktor 2 (Nrf2) aktivering. EDA metoden applicerades sedan för att hitta ämnen som potentiellt driver toxicitet i effluent från avloppsreningsverk (WWTP), urban snö, och kommersiellt flaskvatten. Utöver det så undersöktes den för närvarande uppnådda graden av harmonisering inom suspect screening och nontarget screening av hel fiskvävnad genom en interlaboratoriestudie med 16 olika deltagare, baserat på både vätsktekromatografi (LC)-HRMS och gaskromatografi (GC)-HRMS. Östrogen aktivitet detekterades i WWTP-effluenten, och det urbana snöprovet som härstammade från en fotbollsplan med konstrgräs. Ursprunget till aktiviteten kunde bara föreslås med osäkerhet, och ett behov av ökad känslighet hos HRMS metoder i EDA framlyfts. AhR-aktivitet detekterades i WWTP-effluenten och i de två urbana snöproverna, och Nrf2-aktivitet i WWTP-effluenten. Både AhRoch Nrf2-aktiviteten försvann dock när proven fraktionerades. Av de ämnen som identifierades med högre säkerhet i WWTP-effluenten kunde 60 % detekteras även i åvattnet hos den mottagande ån nedströms effluentutsläppet, medan Interlaboratoriestudien på fiskvävnad visade att det fanns en stor variation mellan target-, suspect- och non-target screeningar som utförts av olika laboratorier. Skillnaden verkade inte bero på olika metoder för provupparbetning utan på andra faktorer. Fortsatta ansträngningar för förbättrad harmonisering är nödvändiga för att uppnå mer jämförbara studier i framtiden.

Bidragets översatta titel	Effektdriven analys och suspect screening för att identifiera potentiellt toxicitetdrivande ämnen i vatten
Originalspråk	Engelska
Kvalifikation	Doktor i filosofi
Förlag	Swedish University of Agricultural Sciences
Tryckta ISBN	978-91-8124-057-3
Elektroniska ISBN	978-91-8124-103-7
DOI	https://doi.org/10.54612/a.5uaek3dad6
Status	Publicerad - 2025

Nyckelord

Effect-directed analysis
bottled water
high-resolution mass spectrometry
highthroughput fractionation
suspect screening
urban snow
wastewater treatment plant effluent
whole fish tissue

SLU-serie

Acta Universitatis Agriculturae Sueciae

Åtkomst av dokument

10.54612/a.5uaek3dad6

FulltextSlutlig publicerad version, 8,09 MBLicens: CC BY-NC-ND

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abstract = "A method for effect-directed analysis (EDA) was developed using the novel technique of high-throughput fractionation in combination with ultra-high pressure liquid chromatography high-resolution mass spectrometry (UPLC-HRMS) and a bioassay battery targeting four different endpoints. The endpoints included the estrogen receptor (ER), androgen receptor (AR), aryl hydrocarbon receptor (AhR) and nuclear factor erythroid 2-related factor 2 (Nrf2). The EDA method was applied to wastewater treatment plant (WWTP) effluent, urban snow, and commercial bottled water to identify potential toxic drivers. Additionally, the currently achievable harmonisation of suspect screening and non-target screening of fish biota was investigated in an interlaboratory study across 16 laboratories using both liquid chromatography (LC)-HRMS and gas chromatography (GC)-HRMS. Estrogenic activity was detected for WWTP effluent and one urban snow sample originating from an artificial football field. The sources of the activity could only be suggested with limited certainty, underscoring the need for higher sensitivity of HRMS methods in EDA. AhR activity was detected for the WWTP effluent and two urban snow samples, and Nrf2 activity was found only in the WWTP effluent. However, upon fractionation both the AhR and Nrf2 activities were lost. Of compounds identified with greater confidence in WWTP effluent, 60 \% were detected downstream of the effluent discharge point, while The interlaboratory study on fish biota showed that there was a large variation between target, suspect and non-target screening results across participating laboratories. The differences seemed to be unrelated to sample preparation method, but instead be due to differences in HRMS workflow strategies. Further harmonisation efforts are necessary to improve comparability and reliability in future screenings.",

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N2 - A method for effect-directed analysis (EDA) was developed using the novel technique of high-throughput fractionation in combination with ultra-high pressure liquid chromatography high-resolution mass spectrometry (UPLC-HRMS) and a bioassay battery targeting four different endpoints. The endpoints included the estrogen receptor (ER), androgen receptor (AR), aryl hydrocarbon receptor (AhR) and nuclear factor erythroid 2-related factor 2 (Nrf2). The EDA method was applied to wastewater treatment plant (WWTP) effluent, urban snow, and commercial bottled water to identify potential toxic drivers. Additionally, the currently achievable harmonisation of suspect screening and non-target screening of fish biota was investigated in an interlaboratory study across 16 laboratories using both liquid chromatography (LC)-HRMS and gas chromatography (GC)-HRMS. Estrogenic activity was detected for WWTP effluent and one urban snow sample originating from an artificial football field. The sources of the activity could only be suggested with limited certainty, underscoring the need for higher sensitivity of HRMS methods in EDA. AhR activity was detected for the WWTP effluent and two urban snow samples, and Nrf2 activity was found only in the WWTP effluent. However, upon fractionation both the AhR and Nrf2 activities were lost. Of compounds identified with greater confidence in WWTP effluent, 60 % were detected downstream of the effluent discharge point, while The interlaboratory study on fish biota showed that there was a large variation between target, suspect and non-target screening results across participating laboratories. The differences seemed to be unrelated to sample preparation method, but instead be due to differences in HRMS workflow strategies. Further harmonisation efforts are necessary to improve comparability and reliability in future screenings.

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KW - Effect-directed analysis

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KW - highthroughput fractionation

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KW - urban snow

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KW - whole fish tissue

KW - Effect-directed analysis

KW - bottled water

KW - high-resolution mass spectrometry

KW - highthroughput fractionation

KW - suspect screening

KW - urban snow

KW - wastewater treatment plant effluent

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PB - Swedish University of Agricultural Sciences

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