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5 protocols using prometryn

1

Synthesis and Characterization of Graphene Oxide

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GO was prepared
from graphite flakes, with an average particle
size of 100 meshes, purchased from Sigma Aldrich (graphite, quality
level 100, product no. 332461). Concentrated sulfuric acid (H2SO4, 96%, product no. 30743), sodium nitrate (NaNO3, 99%, product no. 221341), potassium permanganate (KMnO4, >99%, product no. 60458), hydrogen peroxide solution
(H2O2, 30%, product no. 95294), and hydrochloric
acid
(HCl, 37%, product no. 30721), atrazine (product no. 45330, PESTANAL),
atraton (product no. 31206, PESTANAL), prometryn (product no. 45636,
PESTANAL) and acetonitrile (product no. 34888, HPLC-grade Chromasolv)
were purchased from Sigma Aldrich (St Louis, MO). All of the aqueous
solutions were prepared using ultrapure MilliQ distilled water (Millipore,
Bedford, MA).
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2

Synthesis and characterization of nitrate-based compounds

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Phosphoric acid (85 wt% in H2O), urea (99%), glucose, (99%), sodium hydroxide, ethanol (99%) methanol, hexane, and chloroform were purchased from PANREAC, S.A.U. (Barcelona, Spain). Ethylenediaminetetraacetic acid (99%), calcium nitrate tetrahydrate (≥99%), sodium nitrate (≥99%), magnesium nitrate (98%), cobalt(ii) nitrate hexahydrate (98%), terbutryn, prometryn and simetryn were supplied from Sigma-Aldrich (Madrid, Spain). Ultrapure water was obtained through Millipore system for high purification.
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3

Analytical Standards for Environmental and Forensic Analysis

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Materials. HPLC-grade acetonitrile, water, hexafluorobenzene (99%) and chlorobenzene (99.9%), iodobenzene (>99%) and fluorobenzene (>99.5%) were obtained from Sigma-Aldrich (Buchs, Switzerland), and toluene (99.85%) and acetone (99.9%) from Acros Organics (Geel, Belgium). Analytical-grade pesticide and drug standards were purchased from Sigma-Aldrich, and were: ametryn, atrazine, prometon, prometryn, propazine, simazine, terbutryn, disulfoton, famphur, parathion, parathion-methyl, phorate, sulfotep, thionazin, triethyl thiophosphate, dimethoate, metolachlor, pyrimethanil, malathion, cyprodinil, flusilazole, cyproconazole, trifloxystrobin, quinoxyfen, tebuconazole, pyriproxyfen, pyridaben, difenoconazole, azoxystrobin, diazepam, cocaine, methadone, desipramine, imipramine, MDMA, ketamine, lidocaine and fentanyl. Phenanthrene-d10, pyrene-d10, and a polycyclic aromatic hydrocarbon mix (CRM 47930) were purchased from Sigma-Aldrich.
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4

Pesticide Standards Preparation and Characterization

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Atrazine, Atrazine-desethyl (DEA), Atrazine-desisopropyl (DIA), bromacil, carbendazim, chlorpyrifos, diuron, imazalil, linuron, metolachlor, prometryn, simazine, terbumeton, terbumeton-desethyl (TED) , terbuthylazine, terbuthylazine-desethyl (TD), terbutryn, thiabendazole, 3,4-dichloroaniline (3,4-DCA), 3,5,6-trichloro-2-pyridinol (TCP) were purchased from Sigma-Aldrich (Madrid, Spain), with a purity higher than 97%. The list of pesticides and TPs available for this study, as well as some physicochemical properties, are listed in Supplementary Material (Table SM1).
HPLC-grade methanol (MeOH), acetone (pesticide residue analysis quality) and formic acid (98-100%, LC-MS grade), were supplied by Scharlau S.L (Barcelona, Spain).
HPLC-grade water (resistivity of 18 MΩ cm) was obtained by purifying demineralised water (Millipore Ltd., Bedford, MA, USA).
Standard stock solutions (500 mg L -1 ) of each compound (except carbendazim) were prepared by dissolving 25 mg (±0.01 mg) of each solid compound in 50 mL of acetone considering the purity of each solid standard. Standard stock solution of carbendazim was prepared in MeOH. Individual stock solutions and working standard solutions were stored at -20 and 4℃ in the dark, respectively.
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5

Pesticide Residue Analysis in Grape Juice

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Materials. HPLC-grade water and acetonitrile and dimethyldichlorosilane (DMDCS, 5% in toluene) were obtained from Sigma-Aldrich (Buchs, Switzerland). PESTANAL© analyticalgrade standards were purchased from Sigma-Aldrich: famphur, parathion, parathion-met, sulfotep, thionazin, ametryn, atrazine, atrazine-D 5 , metolachlor, prometon, prometryn, terbutryn, propazine, simazine, pyrimethanil, cyproconazole, quinoxyfen, flusilazole, trifloxystrobin, azoxystrobin, pyridaben, pyraclostrobin, pyriproxyfen, tebuconazole, cyprodinil, difenoconazole and malathion. Organic grape juice was purchased at local grocery stores in Zurich (Switzerland) and in Waterloo (ON, Canada). PDMS/DVB/PDMS coatings were prepared in-house following the procedure described by Souza-Silva et al. 16 Sample preparation. Individual pesticide standard stock solutions were prepared at a concentration of 5 mg/mL in acetonitrile, and stored at -20 °C. A mix of the pesticides at 100 µg/mL in acetonitrile was prepared from the stock solutions. Diluted solutions used for SPME analysis were prepared in ACN from the mix and were stored at a temperature of 4 °C.
The grape juice samples were spiked with an aliquot of the pesticides standards mixtures, always keeping the total amount of solvent spiked in the matrix below 1% (v:v).
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