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9 protocols using dichloromethane

1

Felodipine Solubility Enhancement Formulation

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Felodipine (Fel) was purchased from Chemshuttle (Jiangsu, China). Polyvinylpyrrolidone/vinyl acetate (PVPVA, Kollidon VA 64) was obtained from the BASF Corporation (Ludwigshafen, Germany). d-α-tocopheryl polyethylene glycol 1000 succinate (TPGS) was purchased from Sigma-Aldrich (St. Louis, MO, USA). Methanol and dichloromethane were purchased from Mallinckrodt Baker (Phillipsburg, NJ, USA). The aqueous media used in all experiments was kept constant, i.e., 100 mM pH 6.8 phosphate buffer, which was prepared by dissolving 7.06 g of monosodium phosphate monohydrate and 6.94 g of sodium phosphate dibasic anhydrous in 1 L of deionized water.
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2

Analytical Grade Chemical Preparation

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The chemicals used were analytical grade. Chemical such as dichloromethane (DCM) from Mallinckrodt Baker (Phillipsburg, NJ, USA); n-hexane was purchased from Tedia (Fairfield, OH, USA); Silica gel 60 PF254 (MERCK, Germany); anhydrous sodium sulfate (Rochelle Chemicals, USA). Prior to use, all glass-ware and sample bottles for trace or organic analysis were washed in a liquid detergent solution, rinsed with a pure acetone and n-hexane mixture, and then heated in an oven at 120 °C for 12 h (Isioma and Lawrence, 2015 (link)). Sigma-Aldrich provided reference grade pesticide standards with purity ranging from 98.5 to 99.5 percent (CRM47426 Johannesburg, South Africa).
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3

Synthesis and Characterization of Pyridyl Porphyrins

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meso-Tetrakis(2-N-pyridyl)porphyrin (H2T-2-PyP) and meso-tetrakis(3-N-pyridyl)porphyrin (H2T-3-PyP) were purchased from Frontier
Scientific. Ethyl p-toluenesulfonate (98%) was from
Sigma-Aldrich. The n-octyl p-toluenesulfonate
and methyl-tri-n-octylammonium chloride (>95%) were from TCI America.
MnCl2·4H2O (99.7%) was supplied by J. T.
Baker, FeCl2 (98%) was from Sigma-Aldrich, and NH4PF6 (99.99%) was from GFS chemicals. Anhydrous diethyl
ether and acetone were from EMD chemicals, while dichloromethane,
chloroform, acetonitrile, EDTA, and KNO3 were purchased
from Mallinckrodt. Anhydrous N,N-dimethylformamide
(DMF) of 99.8% purity (kept over 4-Å molecular sieves) and plastic-backed
silica gel TLC plates (Z122777-25EA) were from Sigma-Aldrich. Xanthine,
equine ferricytochrome c (lot 7752), and (+)-sodium l-ascorbate (>98%) were from Sigma, whereas xanthine oxidase
was prepared by R. Wiley.1 (link) Triethylamine
(Et3N) of >99.5% purity was obtained from Thermo Scientific
Pierce. All chemicals were used as received without further purification.
The 1H NMR spectra were recorded on a spectrometer “Mercury
Varian 300” with deuterated chloroform as solvent.
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4

Chondroprotective Kartogenin Biomaterial

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The chemicals used in the work, such as 2-[(Biphenyl-4-yl)carbamoyl]benzoic acid(Kartogenin, KGN) (Sigma-Aldrich Company, United Kingdom), 1-Dodecanol (Alfa Aesarm, United States), ε-caprolactone (Alfa Aesarm, United States), methoxyl PEG hydrazide 5k (NANOCS, United States), petrol (Sigma-Aldrich Company, United Kingdom), stannous octanoate (Sigma-Aldrich Company, United Kingdom), acetonitrile (ACN) (Sigma-Aldrich Company, United Kingdom), ether (J.T.Baker, United States), pyrene (Sigma-Aldrich Company, United Kingdom), dichloromethane (Mallinckrodt, United States), Dess-Martin periodinane (solution in 0.3M dichloromethane) (Sigma-Aldrich Company, United Kingdom), dimethyl sulfoxide (Sigma-Aldrich Company, United Kingdom), and ethanol (Merck, Germany).
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5

Emu Oil Fatty Acid Composition Analysis

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Pharmaceutical grade pure Emu oil was purchased from ClinicReady, Queensland, Australia. The fatty acid composition of the emu oil consists mainly of oleic (51.6%) and palmitic (22.5%) acid. Dichloromethane, Acetonitrile, Ethanol, Isopropy Alcohol (IPA), and DMSO were supplied by Mallinckrodt Chemicals, Bedminster, NJ, USA. All other chemicals and reagents used in the study were of analytical grade and purchased of commercial sources.
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6

Ochratoxin A Detection in Food Samples

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Acetonitrile and methanol (both HPLC grade) were purchased from Carlo Erba Reagents (Milan, Italy). Dichloromethane and hydrochloric acid (both HPLC grade) were purchased from Mallinckrodt Baker (Milan, Italy). Ultrapure water was produced by a Millipore Milli-Q system (Millipore, Bedford, MA). Ochratoxin A (OTA), sodium chloride (NaCl, ACS grade), sodium hydrogen carbonate (NaHCO3, ACS grade), Tween 20, and acetic acid were purchased from Sigma-Aldrich (Milan, Italy). OTA immunoaffinity columns (OchraTest™) were obtained from VICAM, A Waters Business (Milford, MA). Glass microfiber filters (GF/A) and paper filters (No. 4) were purchased from Whatman (Maidstone, UK). OTA immunoaffinity columns (OchraPrep®) and ELISA test kits (RIDASCREEN® Ochratoxin A 30/15) were purchased from R-Biopharm (R-Biopharm AG, Darmstadt, Germany).
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7

HPLC-MS/MS Analysis of Oxcarbazepine and Metabolite

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Oxcarbazepine (99.6%) was purchased from USP (Rockville, USA) and the racemic MHD metabolite (98%) from Toronto Research Chemicals (North York, Canada). 4-Methylprimidone (internal standard, IS) was purchased from Sigma (St.
Louis, MO, USA). The solvents dichloromethane and tert-butyl methyl ether were obtained from Mallinckrodt Baker (Phillipsburg, NJ, USA), hexane, methanol and ethanol from Panreac Química SAL (Barcelona, Spain), and isopropanol from Tedia Way (Fairfield, USA). All solvents were of chromatographic grade. Ammonium acetate was obtained from Mallinckrodt Baker (Phillipsburg, Xalostoc, Mexico). The water used in the experiment was purified with the Sinergy UV ® system (Millipore, Molsheim, France).
Stock solutions were prepared in methanol at a concentration of 100 g OXC/mL and 200 g MHD/mL. Dilutions were then prepared to obtain the working solutions at concentrations of 0.008, 0.02, 0.04, 0.2, 0.4, 0.8, 1.6, 2.4 and 4 g OXC/mL methanol and of 0.08, 0.2, 0.4, 2.0, 4.0, 8.0, 16, 24 and 40 g MHD/mL methanol. The 4methylprimidone solution was prepared at a concentration of 200 g/mL methanol and diluted to 40 g/mL.
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8

Ochratoxin A Extraction and HPLC Analysis

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The chemicals and solvents used for OTA extraction and for HPLC analysis were analytical grade or HPLC grade. The OTA standard used to prepare standard solutions for the validation of the applied methodology was obtained from Sigma-Aldrich Co. (St. Louis, MO, USA). Immunoaffinity columns used for samples purification (OchraTest™ WB) were purchased from Vicam® (Milford, MA, USA). PBS buffer pH 7.0 used during sample clean up procedure was prepared by dissolving sodium chloride (8.0 g), sodium phosphate dibasic (1.2 g), potassium phosphate monobasic (0.2 g), and potassium chloride (0.2 g) in purified water so as to obtain 1 litre of buffer. Water, acetonitrile, isopropyl alcohol, dichloromethane, and methanol were purchased from Mallinckrodt Baker B.V. (Deventer, The Netherlands); citric acid, phosphoric acid, sodium bicarbonate, sodium chloride, sodium phosphate dibasic, potassium phosphate monobasic, and potassium chloride were purchased from Carlo Erba Reagents (Cornaredo, MI, Italy); acetic acid and ethyl acetate were obtained from Sigma-Aldrich Co. (St Louis, MO, USA).
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9

Formulation and Characterization of Lopinavir

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Lopinavir was purchased from Chemshuttle (Wuxi, China). HPMCAS (HF grade) and HPMCP polymers were obtained from Shin-Etsu (Tokyo, Japan). HPMC (Methocel E5) and ethylcellulose NF (Ethocel) were obtained from the Dow Chemical Company (Midland, MI). Cellulose acetate (40% acetyl groups) and cellulose acetate phthalate were obtained from Fluka (Honeywell Specialty Chemicals Seelze GmbH, Seelze, Germany). Eudragit® RL PO was obtained from Röhm Pharma Polymers (Röhm GmbH, Sontheim/Brenz, Germany). HPLC grade methanol, acetonenitrile, and dichloromethane were purchased from Mallinckrodt Baker (Phillipsburg NJ). All other chemicals (citric acid and sodium citrate dihydrate) were purchased from SigmaAldrich (St. Louis, MO).
A total amount of 8.215 g citric acid anhydrous and 2.130 g sodium citrate dihydrate were dissolved in water to a final volume of 1000 mL to prepare 50 mM pH 3 citric acid buffer.
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