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. Broussey-en-woevre and . Fossé,

. Manoncourt-sur-seille and . Fossé,

, Diversité floristique sur les 6 années de suivies du site de Manoncourtsur-Seille (relevés effectués en Mai-Juillet), vol.5

, /2016 frozen at -20 °C to analyse for IPU and DMT metabolites (methods B and C), 2011.

, The sample was flushed onto the online Solid Phase Extraction (SPE, Oasis HLB 25 ?m, 2.1x20 mm, Waters) with water/methanol (90/10) (v/v) and then elution used a gradient of methanol and distilled water in the Kinetex C18 2.6 µm (4.6x100 mm), Phenomenex. The limits of quantification (LOQ) were 5.0, 4.9, 10.3 and 10.4 ?g.L -1 for BSC, CYP, IPU and DMT, respectively. Methods B and C were done on an Acquity Ultra-Performance Liquid Chromatography system (UPLC, Waters) interfaced to a triple quadrupole mass spectrometer (Quattro Premier XE, Waters). Method B analysed mono-desmethyl, Method A used liquid chromatography on an Ultimate 3000 RSLC system and Diode Array Detector 20

, Elution used a gradient of acidified water and acidified acetonitrile (0.05% Acid Formic -AF) in the Kinetex 1.7 µm C18 100A (100x2.1 mm), Phenomenex. The LOQ were 0.02 µg.L -1 for CGA 39981 and CGA 42443, 0.025 µg.L -1 for MD-IPU and 0.05 µg.L -1 for DD-IPU. Method C analysed DMT metabolite CGA 42443 (DMT-OA), DMT metabolite CGA 354742 (DMT-ESA), DMT metabolite CGA 369873, DMT metabolite CGA 373464, DMT metabolite SYN 530561 and DMT metabolite SYN 528702. The sample was flushed onto the online SPE cartouche (Oasis HLB 25 µm, 2.1x20 mm, Waters) with acidified water, metabolite CGA 39981 and DMT metabolite CGA 42443. The sample was flushed onto the online SPE cartouche (Oasis HLB 25 µm, 2.1x20 mm, Waters) with water (neutral pH), p.7

. Af, using Chromeleon® software (V 6.80). Cl -and Br -concentrations were analysed using an AS20 guard column (4x50 mm), followed by a polymeric AS20 analytical column (4x250 mm), Certified standard solutions from Inorganic Ventures

, Sediments were freeze-dried, manually crushed and homogenized, before their extraction by

(. Quechers, . Quick, . Easy, . Cheap, and . Effective, QuECHERS extractions were performed according the modified method of Fernandes et al. (2013) 26 in five steps: (1) 1.0 ± 0.02 g of sediment was placed in a 50 mL polypropylene centrifuge tube, and 1 mL of water was added

, After 1 h of moistening, 10 mL of acetonitrile was added, and the tubes were vortexed for 30 s

, Extraction salts were added, 4 g MgSO 4 , 1 g NaCl, 1 g Na 3 citrate,2H 2 O and 0.5 g Na 2 citrate,1,5H 2 O, shaken vigorously for 30 s and then vortexed for 15 s, sonicated for 5 min (50/60 Hz, 100 W) and centrifuged for 5 min at 3000xg

, 5 mL of the supernatant was purified with150 mg MgSO4 and 50 mg PSA, vortexed for 15 s and centrifuged for 5 min at 3000xg

, 3 mL of the supernatant was transferred in a glass vial and evaporated dry under N 2 flux. The residues were resuspended with 10 mL of water before analysis. respectively for BSC, CYP, DMT and IPU. The efficiencies were determined in

, QuECHERS extractions were performed according the modified method of Fernandes et al. (2013) 26 in 5 steps: (1) a portion of 1.0 ± 0.02 g of sediment was placed into a 50 mL polypropylene centrifuge tube

, ) after 1 h of moistening, 10 mL of acetonitrile was added, and the tubes were vortexed for 30 s

, ) the extraction salts were added (4 g of MgSO 4 , 1 g of NaCl, 1 g of Na 3 citrate,2H 2 O and 0.5 g of Na 2 citrate,1,5H 2 O, agitated vigorously for 30 s and then vortexed for 15 s, sonicated for 5 min (50/60 Hz, 100 W) and centrifuged for 5 min at 3000xg

, 5 mL of the supernatant was purified with150 mg of MgSO4 and 50 mg of PSA, vortexed for 15 s and centrifuged for 5 min at 3000xg

, 3 mL of the supernatant was transferred in a glass vial and evaporated dry under N 2 flux. The residues were resuspended with 10 mL of water before analysis. respectively for BSC, CYP, DMT and IPU. The efficiencies were determined in triplicate

, 20 g of sediments were spiked with 20 mL of a solution at 10 mg.L -1 containing the 4 pesticides and under agitation for 5 days. Then, sediments were centrifuged at 3500 rpm and the supernatant was analyzed (i.e. to know the real amount of pesticides in sediments) while sediments were frozen at -20°C