Effect monitoring of selected effluents and receiving ...€¦ · Effect monitoring of selected...

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Effect monitoring of selected effluents and receiving waterbodies in the Meuse and Scheldt basins: overall toxicity and endocrine disruption assessment. Yves Marneffe & Carole Chalon ISSeP (Institut Scientifique de Service Public) - Cellules Ecotoxicologie et Qualité des eaux, rue du Chéra, 200, 4000 Liège, Belgium ([email protected]) Materials and methods Acknowledgements : The DGO3 of Wallonia supports the network. We thank J.F. Vaerewyck and J. Delvaux for the fruitful exchanges. A study was carried out with complementary tools in different rivers of the Meuse and Scheldt basins, upstream, downstream and in the effluent of selected industries and urban wastewater treatment plants. An active monitoring using laboratory bioassays was carried out, combining ecotoxicological and physico-chemical measurements. Besides a standard battery of bioassays, a special attention was paid to the presence of endocrine disrupting compounds. Indeed, in wastewaters and surface waters, they have become a major concern worldwide, since they negatively affect wildlife and humans. A yeast estrogen screen (YES) assay was conducted as effective first-tier screening tool to assess the estrogenic potential of surface water or effluent samples. Introduction Results and discussions Conclusion One third of the studied effluents exhibited high estrogenic activity levels and two third an important overall toxicity. These effluents are directly discharged in surface water bodies and the results indicate a higher vulnerability of the small rivers with higher estrogenicity levels than in the large ones. 50 % of the surface water samples showed estrogen equivalency above the concentration (4 ngE2/L) that feminizes fathead minnows (Lange et al. 2001). The results obtained on water samples were in good accordance with the measurements in POCIS extracts (between 40 and 80 ng E2 eq/POCIS in the smaller rivers Haine and Hain and between 6 and 11 ng E2 eq/POCIS in the larger river Meuse). These values are also in good accordance with other studies: Alvarez et al. (2008) found estrogenic activities between 14 and 79 ng E2 eq/POCIS on POCIS placed in two rivers. Vermeirssen et al. (2005) found activities between 2 et 65 ng E2 eq/POCIS on POCIS placed downstream from WWTP in rivers of Switzerland. The qualitative chemical screening on POCIS extracts confirmed the presence of estrogenic compounds. Moreover, we used a battery of short term and chronic bioassays with the bacteria Vibrio fischeri, the alga Pseudokirchneriella subcapitata, the rotifer Brachionus calyciflorus and the microcrustacea Daphnia magna to assess their overall toxicity Polar organic chemical integrative samplers (POCIS) were also used at some locations to sample hydrophilic compounds such as pharmaceuticals, personal care products, hormones, and pesticides having low log n-octanol-water partition coefficents (Kows < 3). POCIS extracts were screened for the presence of estrogenic chemicals using the yeast estrogen screen (YES) assay. Estrogenic activity (surface waters) Yeast estrogen screen test Overall toxicity (effluents) Standard test battery Estrogenic activity (effluents) Yeast estrogen screen test Estrogenic activity (Pocis) Yeast estrogen screen test 36 major industrial discharges and 20 sampling points in the receiving waters (upstream and downstream of the effluent) were sampled in the Meuse and Scheldt basins. The results of the Yeast estrogen screen test show that 17 effluents (50%) exhibited estrogenic activities > 1ngE2 eq/l. Very high estrogenic activities (> 70 ngE2 eq/l) were found in 4 industrial effluents (chemical, pharmaceutical, waste and food industries); 5 other effluents induced estrogenic activity > 5 ngE2 eq/l. Results from the YES indicated important estrogenicity in different small rivers such as River Haine and River Hain (>15 ng eq E2/l), whereas samples collected in more important rivers like the River Meuse showed lower estrogenic activities (<2 ng eq E2/l). The estrogenic activity levels measured in POCIS extracts (between 40 and 80 ng E2 eq/POCIS in the rivers Haine and Hain and between 6 and 11 ng E2 eq/POCIS in the river Meuse) are in good accordance With the differences observed in water samples originating from small and large rivers respectively. Amongst the 36 industrial effluent samples, 3 were classified as extremely toxic (>100 TU50), 6 as very toxic (10-100 TU50), 15 as toxic (1-10 TU50), 2 as weakly toxic (< 1 TU50) and 10 as not toxic (0 TU50). Chemical industry and laundry effluents (galvanizing) were particularly toxic for Daphnia magna, algae and Brachionus calyciflorus (discharge in River Vesdre). Vibrio fischeri appear to be very sensitive to surfactant and waste treatment effluent. Species used in the battery give complementary information Approved and suspected estrogenic compounds were detected in the POCIS extracts (qualitative analyse by gas chromatography/mass spectrometry (GC/MS). Group Substance Peak area ratio downstream/upstream Pharma WWTP1 WWTP2 Waste recycling Plastic monomer Bisphénol A 0.95 1.25 0.8 1.3 Hormone Estrone 0.99 0.77 17β‐estradiol 0.64 Pesticide Triclosan 1.38 1.48 0.81 0.99 CisPropiconazole 0.88 1.2 0.73 1.55 TransPropiconazole 0.84 1.33 0.84 1.36 Atrazine 0.86 1.05 0.98 0.98 Cosmetic preservative Méthylparaben 1.33 Ethylparaben 1.41 Propylparaben 1.29 UV filter Benzophénone1 1.12 0.88 Benzophénone3 1.99

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Page 1: Effect monitoring of selected effluents and receiving ...€¦ · Effect monitoring of selected effluents and receiving waterbodies in the Meuse and Scheldt basins: overall toxicity

Effect monitoring of selected effluents and receiving waterbodies in the Meuse and Scheldt basins: overall toxicity

and endocrine disruption assessment.Yves Marneffe & Carole Chalon

ISSeP (Institut Scientifique de Service Public) - Cellules Ecotoxicologie et Qualité des eaux, rue du Chéra, 200, 4000 Liège, Belgium ([email protected])

Materials and methods

Acknowledgements : The DGO3 of Wallonia supports the network. We thank J.F. Vaerewyck and J. Delvaux for the fruitful exchanges.

A study was carried out with complementary tools in different rivers of the Meuse and Scheldt basins, upstream, downstream and in the effluent of selected industriesand urban wastewater treatment plants. An active monitoring using laboratory bioassays was carried out, combining ecotoxicological and physico-chemicalmeasurements. Besides a standard battery of bioassays, a special attention was paid to the presence of endocrine disrupting compounds. Indeed, in wastewaters andsurface waters, they have become a major concern worldwide, since they negatively affect wildlife and humans.

A yeast estrogen screen (YES)assay was conducted as effectivefirst-tier screening tool to assess theestrogenic potential of surface wateror effluent samples.

Introduction

Results and discussions

Conclusion

One third of the studied effluents exhibited high estrogenic activity levels and two third an important overall toxicity. These effluents are directly discharged in surfacewater bodies and the results indicate a higher vulnerability of the small rivers with higher estrogenicity levels than in the large ones. 50 % of the surface water samplesshowed estrogen equivalency above the concentration (4 ngE2/L) that feminizes fathead minnows (Lange et al. 2001). The results obtained on water samples were ingood accordance with the measurements in POCIS extracts (between 40 and 80 ng E2 eq/POCIS in the smaller rivers Haine and Hain and between 6 and 11 ng E2eq/POCIS in the larger river Meuse). These values are also in good accordance with other studies: Alvarez et al. (2008) found estrogenic activities between 14 and 79 ngE2 eq/POCIS on POCIS placed in two rivers. Vermeirssen et al. (2005) found activities between 2 et 65 ng E2 eq/POCIS on POCIS placed downstream from WWTP inrivers of Switzerland. The qualitative chemical screening on POCIS extracts confirmed the presence of estrogenic compounds.

Moreover, we used a battery of short term andchronic bioassays with the bacteria Vibrio fischeri,the alga Pseudokirchneriella subcapitata, the rotiferBrachionus calyciflorus and the microcrustaceaDaphnia magna to assess their overall toxicity

Polar organic chemical integrativesamplers (POCIS) were also used at somelocations to sample hydrophilic compoundssuch as pharmaceuticals, personal careproducts, hormones, and pesticides havinglow log n-octanol-water partition coefficents(Kows < 3). POCIS extracts were screenedfor the presence of estrogenic chemicalsusing the yeast estrogen screen (YES)assay.

Estrogenic activity (surface waters)Yeast estrogen screen test

Overall toxicity (effluents)Standard test battery

Estrogenic activity (effluents)Yeast estrogen screen test

Estrogenic activity (Pocis)Yeast estrogen screen test

36 major industrial discharges and 20 sampling points in the receiving waters (upstream and downstream of the effluent) were sampled in the Meuse and Scheldtbasins.

The results of the Yeast estrogen screen test show that 17 effluents (50%)exhibited estrogenic activities > 1ngE2 eq/l. Very high estrogenic activities (> 70ngE2 eq/l) were found in 4 industrial effluents (chemical, pharmaceutical, wasteand food industries); 5 other effluents induced estrogenic activity > 5 ngE2 eq/l.

Results from the YES indicatedimportant estrogenicity indifferent small rivers such asRiver Haine and River Hain (>15ng eq E2/l), whereas samplescollected in more importantrivers like the River Meuseshowed lower estrogenicactivities (<2 ng eq E2/l). Theestrogenic activity levelsmeasured in POCIS extracts(between 40 and 80 ng E2eq/POCIS in the rivers Haineand Hain and between 6 and 11ng E2 eq/POCIS in the riverMeuse) are in good accordance

With the differences observed in water samples originating from small and large rivers respectively.

Amongst the 36 industrial effluent samples, 3 were classified as extremely toxic(>100 TU50), 6 as very toxic (10-100 TU50), 15 as toxic (1-10 TU50), 2 as weaklytoxic (< 1 TU50) and 10 as not toxic (0 TU50). Chemical industry and laundryeffluents (galvanizing) were particularly toxic for Daphnia magna, algae andBrachionus calyciflorus (discharge in River Vesdre). Vibrio fischeri appear to bevery sensitive to surfactant and waste treatment effluent. Species used in thebattery give complementary information

Approved and suspectedestrogenic compoundswere detected in thePOCIS extracts (qualitativeanalyse by gaschromatography/massspectrometry (GC/MS).

Group Substance Peak area ratio downstream/upstream

Pharma WWTP‐1 WWTP‐2Waste 

recycling

Plastic monomer Bisphénol A 0.95 1.25 0.8 1.3

HormoneEstrone 0.99 ‐ 0.77 ‐

17β‐estradiol ‐ ‐ 0.64 ‐

Pesticide

Triclosan 1.38 1.48 0.81 0.99

Cis‐Propiconazole 0.88 1.2 0.73 1.55

Trans‐Propiconazole

0.84 1.33 0.84 1.36

Atrazine 0.86 1.05 0.98 0.98

Cosmetic preservative

Méthylparaben 1.33 ‐ ‐ ‐

Ethylparaben 1.41 ‐ ‐ ‐

Propylparaben 1.29 ‐ ‐ ‐

UV filterBenzophénone‐1 1.12 ‐ ‐ 0.88

Benzophénone‐3 1.99 ‐ ‐ ‐