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10 protocols using ortho phosphoric acid

1

Synthesis of Endocrine-Disrupting Compounds

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The reagents used in this work are described in the following list:

Androsterone 97,7%, Sigma Aldrich, CAS Number: 53–41-8.

Bisphenol A 99,5%, Dr Ehrenstorfer, CAS Number: 80–05-7.

Estrone 99,3%, Sigma Aldrich, CAS Number: 53–16-7.

Graphite powder, BAYCARBON Inc., Product SP-1.

Hydrochloric Acid, Sigma Aldrich, CAS Number: 7647–01-0.

Hydrogen Peroxide, Chem-Lab, CAS Number: 7722–84-1.

Nitric Acid, Sigma Aldrich, CAS Number: 7697–37-2.

19-Norethindrone 99.6%, Sigma Aldrich, CAS Number: 68–22-4.

Orthophosphoric Acid, Scharlau, CAS Number: 7664–38-2.

Potassium Bromide, Fluka, CAS Number: 7758–02-3.

Potassium Permanganate, Merck, CAS Number: 7722–64-7.

Sulfuric Acid, Sigma Aldrich, CAS Number: 7664–93-9.

Vanadium Pentoxide, Merck, CAS Number: 1314–62-1.

17α-Ethinylestradiol 99,5%, Dr Ehrenstorfer, CAS Number: 57–63-6.

2,4-Dichlorophenol 99,7%, Supelco, CAS Number: 120–83-2.

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2

HPLC Analysis of Extracted Compounds

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All solvents used were HPLC grade, and all reagents were analytical grade. The analysis was performed using a high-performance liquid chromatography system (Hitachi D2000), which consisted of an L-2130 HTA Pump, an L-2200 autosampler, and an L-2455 diode array detector. The extracted compound was separated using an Inertsil ODS-2 C18 column (250 mm × 4.6 mm, 5 μm) with a gradient mobile phase of 0.3% ortho-phosphoric acid (Scharlab) in ddH2O (solvent A) and acetonitrile (Fisher Chemical) (solvent B). HPLC was performed at a flow rate of 0.8 ml/min with detection at 220 nm. The column temperature was maintained at 30°C. All samples were diluted in methanol (Honeywell) before analysis. Chromatographic peaks were identified on the basis of retention time.
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3

Screening Antioxidant Capacity of Onion Extracts

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For the film preparation, medium-sized yellow onion bulbs in commercial stages were acquired from markets in the city of São Carlos, São Paulo, Brazil. For the incorporation of clay, Laponite XLG (Na0.7[(Mg5.5Li0.3)Si8O20(OH)4]) obtained from BYK-Chemie was used for clay incorporation. Milli-Q® water, sodium salicylate (CAS 54-21-7, 99.5%), 2,5-dihydroxybenzoic acid (CAS 490-79-9, 99%) from Sigma-Aldrich, HPLC-grade methanol (CAS 67-56-1), hydrogen peroxide (CAS 7722-84-1, 30%) and orthophosphoric acid (7664-38-2, 84%) from Scharlab were used for the antioxidant assay.
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4

Quantifying NSAID Metabolite Profiles

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The NSAIDs diclofenac (sodium salt, D6899, DIC), ketoprofen (≥ 98% TLC, K1751, KET), naproxen (≥ 98%, sodium salt, M1275, NAP) and Ibuprofen (sodium salt, ≥ 98% GC, I1892, IBU) were purchased from Sigma-Aldrich. Stocks solutions of 4 mg ml -1 for each NSAIDs were prepared in Methanol (LC-MS grade, Merck). For the confirmation of the metabolites, Prostaglandin E1 (P5515) and Arachidonic acid (23401) standards from Sigma Aldrich were used. Lipid extraction was based on the method of Zöllner and Kirsch (1962) , using Chloroform (HPLC grade, Merck), Methanol (HPLC grade, Sigma Aldrich) for the extraction and for the analysis Vanillin (99%, V1104, Sigma Aldrich) and orthophosphoric acid (85%, reagent grade, Scharlau) were used. The mobile phase used for metabolomics approach was HPLC grade acetonitrile and water purchased from Merck (Darmstadt, Germany).
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5

Synthesis of alpha-cyclodextrin conjugates

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Alpha-cyclodextrin, N,N′-carbonyldiimidazole (CDI), imidazole, and ammonium dihydrogen phosphate were purchased from Sigma Aldrich (St. Louis, MO, USA). Milli Q water was generated using an Ultramatic Wasserlab purification system (Pamplona, Spain). For pH adjustment, 37% hydrochloric acid and 85% ortho-phosphoric acid (Scharlab, Madrid, Spain) were used. Analytical grade acetonitrile was purchased from Honeywell (Charlotte, NC, USA). Bentonites and zeolites were kindly provided by Nurel S.A. (Zaragoza, Spain).
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6

Moroccan Pine Cone-Based Activated Carbon for Bisphenol A Removal

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Moroccan pine cones (Pinus halepensis) were collected locally from a forest in the province of Sefrou, in the Fez-Meknes region, Morocco. Zinc chloride (ZnCl2), and ortho-phosphoric acid, (H3PO4, 85 % w/w.) were purchased from Scharlau (Spain). Bisphenol A (≥99 % purity) was procured from Sigma Aldrich (Germany). Hydrochloric acid (HCl, ≥37 %), and sodium hydroxide (NaOH, ≥97 %) were purchased from Fluka (Germany). Ethanol was supplied by Biosmart (Morocco). Reverse osmosis (RO) water was prepared in the laboratory using an RO purification system (Elettronica Veneta) and used to prepare BPA solutions for adsorption experiments. All reagents were used as received without further purification. Table 1 presents the representative emerging contaminant selected for assessing the performance of the prepared activated carbons for water treatment: Bisphenol A (BPA).

General physicochemical properties of BPA [19 (link)].

Table 1
PropertiesBisphenol A
Molecular FormulaC15H16O2
Chemical structureImage 1
Density (g.cm−3)1.20
Molecular weight (g.mol−1)228.291
Water solubility (mg. L−1)120–300
Dissociation constant, pKa10.29
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7

Screening Antioxidant Capacity of Onion Extracts

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For the film preparation, medium-sized yellow onion bulbs in commercial stages were acquired from markets in the city of São Carlos, São Paulo, Brazil. For the incorporation of clay, Laponite XLG (Na0.7[(Mg5.5Li0.3)Si8O20(OH)4]) obtained from BYK-Chemie was used for clay incorporation. Milli-Q® water, sodium salicylate (CAS 54-21-7, 99.5%), 2,5-dihydroxybenzoic acid (CAS 490-79-9, 99%) from Sigma-Aldrich, HPLC-grade methanol (CAS 67-56-1), hydrogen peroxide (CAS 7722-84-1, 30%) and orthophosphoric acid (7664-38-2, 84%) from Scharlab were used for the antioxidant assay.
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8

Favipiravir Analytical Method Development

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Favipiravir was kindly supplied by Optrix Laboratories private Limited, India. Lamivudine, used as an internal standard (IS), was bought from LGC GmbH, Germany. Potassium dihydrogen phosphate, sodium dihydrogen phosphate, ortho phosphoric acid, acetic acid, ammonium formate and formic acid were purchased from Scharlau, Spain. Methanol and acetonitrile (HPLC grade), Sigma Aldrich, Germany.
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9

Phytochemical Analysis of Licorice Extracts

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CO 2 (99.98 % purity) was supplied from Carburos Metálicos (Madrid, Spain). Ethanol (99.8 % purity), Sodium Carbonate anhydrous (99.5% purity) and Folin-Ciocalteu´s reagent were purchased from Panreac (Barcelona, Spain). Gallic acid standard (> 98% purity), 2,2-Diphenyl-1-pycrilhydrazyl (DPPH, 95% purity), (±)-6-Hydroxy-2,5,7,8tetramethyllchromane-2-carboxylic acid (Trolox, 97% purity), liquiritin, liquiritigenin, isoliquiritigenin, glabridin and glycyrrhizic acid were purchased from Sigma-Aldrich (St. Louis, MO, USA). Orthophosphoric acid (85% purity) was purchased from Scharlab S.L. (Sentmenat, Spain). Acetonitrile (99,8% purity) was purchased from Macron (Poland).
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10

Phytochemical Analysis of Licorice Extracts

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CO 2 (99.98 % purity) was supplied from Carburos Metálicos (Madrid, Spain). Ethanol (99.8 % purity), Sodium Carbonate anhydrous (99.5% purity) and Folin-Ciocalteu´s reagent were purchased from Panreac (Barcelona, Spain). Gallic acid standard (> 98% purity), 2,2-Diphenyl-1-pycrilhydrazyl (DPPH, 95% purity), (±)-6-Hydroxy-2,5,7,8tetramethyllchromane-2-carboxylic acid (Trolox, 97% purity), liquiritin, liquiritigenin, isoliquiritigenin, glabridin and glycyrrhizic acid were purchased from Sigma-Aldrich (St. Louis, MO, USA). Orthophosphoric acid (85% purity) was purchased from Scharlab S.L. (Sentmenat, Spain). Acetonitrile (99,8% purity) was purchased from Macron (Poland).
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