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19 protocols using dimethyl phthalate

1

Quantification of Phthalate Esters in Plastic Bottles

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PET and HDPE bottles were purchased from Iran Petrochemical Co. (Tehran, Iran). A standard solution of phthalic acid esters, containing six compounds (diethyl phthalate (DEP), dimethyl phthalate (DMP), butyl benzyl phthalate (BBP), di-n-octyl phthalate (DNOP), dibutyl phthalate (DBP), and bis (2-ethylhexyl) phthalate (DEHP) at 2.0 mg/mL in n-hexane (purity 99.8%)), was purchased from Sigma-Aldrich (St. Louis, MO, USA). The phthalic acid esters calibration and quality control samples were prepared by serial dilution of the stock solution in methanol-water (50: 50, v/v). Benzyl benzoate (internal standard, IS) was added to each sample at a final concentration of 1 μg/L. A mixture of acetonitrile, isopropanol and water (40:40:20 v/v) was applied as extraction solution. All the stock and working solutions were kept at 4 °C, in the dark until analysis. The magnetic multi-wall carbon nanotube-polydimethylsiloxane nanocomposite (PDMS/MWCNTs-OH) particles were prepared based on a two-step reaction as explained previously [14 (link)].
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2

Phthalate Standards Preparation and Analysis

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All PEs standards including dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), benzyl butyl phthalate (BBP) and bis(2-ethylhexyl) phthalate (DEHP) were purchased from Sigma Aldrich, Germany. The purities of all PEs were >98%. A 1000 μg mL−1 stock standard solution of each standard was prepared in methanol and stored in glass vials at −20 °C. The standard working solution mixtures (0.001–1.00 μg mL−1) were prepared daily by diluting appropriate aliquots of the stock standard solutions to obtain the required concentrations and stored at 4 °C. HPLC grade methanol, acetonitrile and acetone were purchased from Sigma-Aldrich, Germany. Chloroform (CHCl3), dichloromethane (CH2Cl2), chlorobenzene (C6H5Cl), carbon tetrachloride (CCl4) and sodium chloride (NaCl) were from Merck (Darmstadt, Germany). Deionized water (18.2 mΩ cm) was prepared by Pure Lab Ultra water system (ELGA, High Wycombe, UK) and used in all procedures. Glass tight microsyringes (Hamilton, Nevada, USA) were used for measuring the extracted sediment volume and for the DLLME procedure. All glassware used were rinsed with deionized water then acetone before drying at 300 °C for at least 5 hours. Moreover blank runs were done for each set of samples.
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3

Evaluating Ion Source Parameters

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Acenapthene (99%), benzophenone (ReagentPlus®, 99%), cuminaldehyd (≥98%), dimethylphthalate (≥99%), and methyldodecanoate (≥99.5%), as substances for the evaluation of the ion source parameters, were purchased from Sigma-Aldrich (Steinheim, Germany). A multicompound solution (MIX-1) was prepared in methanol (LC-MS Grade) from T. Baker (Giwice, Poland) in a concentration range from 0.1 to 1000 µg/L.
A multiresidue pesticide kit (cat 32562) was purchased from Restek GmbH (Bad Homburg, Germany). It contains organophosphorus (OPP: cat 32563, 32570, 32571), organonitrogen (ONP: cat 32565, 32566, 32567), synthetic pyrethroide (SPP: cat 32568) compounds and herbicide methyl esters (HME: Cat 32569) in toluene (each 100 µg/mL). A multicompound solution of organophosphorus and organonitrogen was prepared. All pesticides were diluted with toluene to a final concentration between 0.1 and 1000 µg/L. Nitrogen and Helium 99.999% were obtained from Air Liquide (Duesseldorf, Germany).
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4

Targeted Analyte Extraction and Quantification

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LC-MS-grade acetonitrile (MeCN) and H2O were purchased from Fluka (Steinheim, Germany). A Milli-Q purification device (Millipore Direct-QR 3, Millipore International, Merck KGaA, Darmstadt, Germany) was used for obtaining the water used in the analyses. Acetone (>99%) and hexane (HPLC grade) were obtained from Centralchem (Bratislava, Slovakia) and VWR Chemicals (Radnor, PA, USA), respectively. Magnesium sulphate (MgSO4), graphitized carbon black (GCB), C18 sorbents, and primary secondary amine (PSA) were supplied by Agilent Technologies (Santa Clara, CA, USA). The aniline standards, namely 3,4-dichloroaniline (3,4-DCA) and 3,5-dichloroaniline (3,5-DCA), were obtained from Riedel de Haën (Seelze, Germany), with purity higher than 99.9%. Phthalate analytical standards, such as dimethyl phthalate (DMP), di-n-butyl phthalate (DnBP), mono-butyl phthalate (mBP), benzyl butyl phthalate (BBP), di-n-octyl phthalate (DnOP), and di-(2-ethyl hexyl) phthalate (DEHP)), were supplied by Sigma Aldrich (Steinheim, Germany).
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5

Standardized Phthalate and Plasticizer Analysis

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The eleven phthalates and the two non-phthalates studied plasticizers are listed in Table 1. Benzyl butyl phthalate (BBP; ≥98%), dibutyl phthalate (DBP; ≥99%), di-cyclohexyl phthalate (DCHP; ≥99%), di(2-ethylhexyl) phthalate (DEHP; ≥99.5%), di-(2-ethylhexyl) terephthalate (DEHT; ≥97%), diethyl phthalate (DEP; ≥99.5%), diethyl phthalate-3,4,5,6-d4 (DEP-d4, IS; ≥98%), diisobutyl phthalate (DIBP; ≥99%), diisononyl phthalate (DINP; ≥99%), dimethyl phthalate (DMP; ≥99%), di-n-octyl phthalate (DNOP; ≥98%), diphenyl phthalate (DphP; ≥99%), dipropyl phthalate (DPP; ≥98%), and tri-octyl trimellitate (TOTM; ≥99%) were purchased from Sigma-Aldrich (Saint-Quentin Fallavier, France). HPLC-grade solvents were used. Acetone, dichloromethane, and acetonitrile were purchased from VWR (Fontenay-sous-Bois, France). Ultra-pure water was supplied by a Milli-Q purification system from Millipore (St Quentin en Yvelines, France).
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6

Graphene Oxide Synthesis and Characterization

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Chromium (III) nitrate nonahydrate, diethyl ether, ethanol, sodium hydroxide pellets, para-benzoquinone, N, O-Bis (trimethylsilyl) acetamide, copper (II) nitrate trihydrate, isopropanol, hydrogen peroxide (30 %), nitric acid, and formic acid were procured from Merck (Germany). Dimethyl phthalate, potassium peroxymonosulfate (PMS), and O-phenylenediamine were supplied by Sigma-Aldrich (USA). GO was provided by Nanografi nanotechnology AS Co. (Turkey). The description of characterization techniques was stated in the supplementary data (Text S1).
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7

Analytical Determination of Pesticides and Phthalates

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Analytical grade dimethyl phthalate, monomethyl phthalate, dibutyl phthalate, dioctyl phthalate, propanil, monalide, chlorpropham, carfentrazone-ethyl, methomyl, 3-chloroaniline, 4-chloroaniline, and 3,4-dichloroaniline were purchased from Sigma-Aldrich (Castle Hill, Australia). Sulfosulfuron, metsulfuron-methyl, pyrazosulfuron-ethyl, imazethpyr, and pendimethalin were gifted by Dow Agrosciences (India). All other chemicals were used at the highest purity available commercially.
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8

Quantification of Biocides and Phthalates

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All reference standards for target compounds were of high purity grade (>99%). Methylisothiazolinone (MI), benzisothiazolinone (BIT), dimethyl phthalate (DMP), diethyl phthalate (DEP), and their internal standards (dimethyl phthalate-3,4,5,6-d4 and diethyl phthalate-3,4,5,6-d4) were obtained from Sigma-Aldrich, methylchloroisothiazolinone (CMI), and its internal standard benzoisothiazol-3-one-13C6 was supplied by Toronto Research Chemicals. Other solvents, including methyl tert-butyl ether (MTBE), were purchased from Duksan Pure Chemicals, South Korea. Dichloromethane (DCM), methanol, and ethyl acetate were purchased from Fisher Scientific Korea Ltd. HPLC grade water was supplied by Avantor Performance Materials Korea. Individual stock solutions of all target compounds and internal standards were prepared in ethanol and stored at −20 °C before use.
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9

Analyzing Phthalate and Alcohol Compounds

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Monobutyl phthalate (MBP, 99% purity), di-n-butyl phthalate (DBP, 99%), diethylhexyl phthalate (DEHP, 99.5%), diethyl phthalate (DEP, 99%), dimethyl phthalate (DMP, 99%), phthalic acid (PA, > 99.5%), 2-ethyl-1-hexanol (99.6%), terephthalic acid (98%), and isophthalic acid (99%) were purchased from Sigma Aldrich Chemie GmbH (Hamburg, Germany). Acetonitrile, ethyl acetate, hexane, and formic acid were of HPLC grade and purchased from Carl Roth (Karlsruhe, Germany).
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10

Phthalate Esters Quantification Protocol

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We obtained dimethyl phthalate (DMP, ≥99%), dibutyl phthalate (DBP, 99%), di-isobutyl phthalate (DIBP, 99%), diethyl phthalate (DEP, 99.5%), and bis (2-ethylhexyl) phthalate (DEHP, ≥99%) from Sigma-Aldrich (Darmstadt, Germany). We purchased HPLC-grade petroleum ether and n-hexane from Merck Chemical Company (Darmstadt, Germany). We obtained analytical-grade H2SO4 (98.3%) from Shengqinghe Chemical Company (Nanjing, China). In addition, dealing with concentrated sulfuric acid and use special acid-resistant gloves and glasses
We used ultrapure water purified using a Millipore Purification System (Burlington, NJ, USA) in all experiments. To minimize the risk of contamination, we used glassware in all experiments, which we strictly washed and checked to ensure the lack of contamination with PAEs before use.
We prepared individual standard stock solutions of each phthalic acid ester (100 mmol L−1) and stored them at 4 °C. We prepared serial dilutions of individual standard stocks and multicomponent solutions containing equal concentrations (100 µmol L−1) of each compound on site by diluting the stock solution with methanol. We constructed calibration curves by plotting the means of triplicate measurements of peak highs against the concentrations of each compound.
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