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495 protocols using dimethylformamide

1

Synthesis of Mannose Triflate-Cysteamine Conjugates

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FDG-MNPs were prepared as described previously.25 Briefly, for the synthesis of mannose triflate-cysteamine, 19.21 mg of mannose triflate (Fluka) was dissolved in 200 μL of distilled water at 90 °C. Separately, 84.85 mg of cysteamine (2-aminoetanethiol; Sigma, Istanbul, Turkey) was dissolved in 70 μL of pure water and adjusted to a pH of 7.5 prior to the addition of 40 mg of NaCNBH3 (Fluka). Both solutions were mixed and heated for 1 hour at 90 °C prior to being precipitated, dried overnight at 65 °C and dissolved in dimethyl formamide (Merck). Next, 100 μL of Kryptofix (Merck) solution (2.0 mg/mL in dimethyl formamide), 200 μL of K2CO3 (Fluka) aqueous solution (2.0 mg/mL), 100 μL of dimethyl formamide (Merkc) and 200 μL of 16 mM NaF (Merck) were added to 1 ml of the prepared mannose triflate-cysteamine (35 mM) and heated for 20 minutes at 90 °C in a water bath. For purification, the product was passed sequentially through a Dowex 50 cation exchange resin column (Sigma), Ambersep 900 quaternary ammonium anion exchange resin (Fluka), Amberlite anion exchange resin (Sigma) and finally a C18 pre-cartridge (Sigma).
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2

Quantification of Phenolic Acids via CEC

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Standards of salicylic acid (1), cinnamic acid (2), syringic acid (3), rosmarinic acid (4), caffeic acid (5) and chlorogenic acid (6) were purchased from Sigma Aldrich (St. Louis, MO, USA); their purity was ≥98%. All solvents (acetonitrile, methanol) and chemicals (ammonium acetate and ammonia) required for CEC analysis had p.A. quality and were bought from Merck Eurolab (Vienna, Austria). Ultrapure water was prepared using a Sartorius arium purification system (Göttingen, Germany).
Chemicals for preparation of the monolith, i.e. 1,4 butanedione, 1-propanol, 2,2-diphenyl-1-picryl-hydrazyl, 3-(trimethoxysilyl) propyl methacrylate, dimethylformamide, allylimidazole, 1,3-propanesultone, dimethylformamide, 2,2-dimethoxy-2-phenylacetophenone and ethyleneglycol dimethacrylate were also obtained from Sigma Aldrich.
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3

Fabrication of PVDF Nanofibers for Energy Conversion

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PVDF solution (20%) was prepared by dissolving 2 g PVDF pellets (MW 275,000 g mol−1, Sigma-Aldrich) in 10 ml solvent mixture of dimethylformamide (Sigma-Aldrich) and acetone (Sigma-Aldrich) (volume ratio of dimethylformamide and acetone, 4/6) and heated at 70 °C for 2 h. To examine the effect of fibre diameter on energy conversion, PVDF nanofibres with different diameters were prepared from PVDF solutions with the concentration ranging from 16 to 28%. The homogeneous PVDF solution was placed to a plastic syringe with a metal needle (21 gauge). A syringe pump (KD Scientific) was used to control the flow rate at 1 ml h−1 and 15 kV high voltage was applied to the syringe needle using a high-voltage power supply (Gamma High Voltage). A grounded rotating drum collector (100 r.p.m.) placed 15 cm away from the needle tip was used for collecting the PVDF nanofibres.
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4

Quantification of Phenolic Acids via CEC

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Standards of salicylic acid (1), cinnamic acid (2), syringic acid (3), rosmarinic acid (4), caffeic acid (5) and chlorogenic acid (6) were purchased from Sigma Aldrich (St. Louis, MO, USA); their purity was ≥98%. All solvents (acetonitrile, methanol) and chemicals (ammonium acetate and ammonia) required for CEC analysis had p.A. quality and were bought from Merck Eurolab (Vienna, Austria). Ultrapure water was prepared using a Sartorius arium purification system (Göttingen, Germany).
Chemicals for preparation of the monolith, i.e. 1,4 butanedione, 1-propanol, 2,2-diphenyl-1-picryl-hydrazyl, 3-(trimethoxysilyl) propyl methacrylate, dimethylformamide, allylimidazole, 1,3-propanesultone, dimethylformamide, 2,2-dimethoxy-2-phenylacetophenone and ethyleneglycol dimethacrylate were also obtained from Sigma Aldrich.
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5

Cobalt-based Metal-Organic Framework Synthesis

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All chemicals were used as received without further purification. Cobalt nitrate hexahydrate [Co(NO3)2.6H2O, 98%], terephthalic acid (1,4-BDC, 98%), and dimethylformamide (DMF, 99.8%) were purchased from Millipore Sigma. Isopropanol (2-propanol, 99.9%) was purchased from Fisher Scientific.
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6

Extraction and Derivatization of Flavonoids

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High purity grade lithium hydroxide monohydrate, esterase, acetone, ethyl chloroacetate, ethyl acetate, dimethylformamide, sodium cholate, anhydrous potassium carbonate, hydrochloric acid, formic acid, acetic acid, amylase, thionyl chloride, ammonia solution, hexane, sodium bicarbonate, phosphate-buffered saline (PBS) buffer, sodium chloride, sodium sulfate, potassium iodide, dichloromethane, dialysis tubing, porcine pancreatin, silica gel, dimethyl sulfoxide, acetonitrile, porcine pepsin, 2-chloroacetamide, and 1,2-dibromoethane were purchased from Millipore Sigma (Burlington, MA, USA). The high purity grade apigenin, quercetin and luteolin were obtained from Indofine chemical company (Hillsborough, NJ, USA).
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7

Synthesis of Modified Amino Acids

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Fmoc-protected
α-amino acids (other than olefinic amino acid Fmoc-(S)-2-amino-2-methyl-hept-6-enoic
acid ((Fmoc-S5-OH)), which was purchased from Sigma-Aldrich) were
purchased from ChemImpex. Rink Amide MBHA resin was purchased from
Sigma-Aldrich. Dimethylformamide (DMF), N,N-diisopropylethylamine (DIEA), acetic anhydride, trifluoroacetic
acid (TFA), dichloromethane (DCM), anisole, 1,2-dichloroethane (DCE),
triisopropylsilane (TIPS), fluorescein isothiocyanate isomer 1 (FITC),
biotin-OSu, and piperidine were purchased from Millipore Sigma and
used as supplied. The Grubbs first-generation catalyst was obtained
from Sigma-Aldrich.
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8

Flavonoids Synthesis and Characterization

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High purity flavonoids, quercetin, apigenin, luteolin, fisetin, kaempferol (Indofine Chemical Company, Hillsborough, NJ, USA), and ethyl chloroacetate, dimethylformamide, anhydrous potassium carbonate, lithium hydroxide, hydrochloric acid, ethyl acetate, thionyl chloride, acetone, ammonia solution, hexane, silica gel, sodium bicarbonate, sodium chloride, sodium sulfate, sodium cholate, porcine pepsin, dialysis tubing, amylase, esterase, porcine pancreatin, dimethyl sulfoxide, and phosphate-buffered saline were purchased from Millipore Sigma (Burlington, MA, USA).
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9

Synthesis and Characterization of Flavonoids

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High purity quercetin and apigenin were purchased from Indofine Chemical Company, Hillsborough, NJ, USA. Ethyl chloroacetate, dimethylformamide, thionyl chloride, lithium hydroxide monohydrate, anhydrous potassium carbonate, sodium chloride, ethyl acetate, hexane, acetone, ammonia solution, silica gel, methyl sulfoxide-d6, sodium bicarbonate, and anhydrous sodium sulfate were purchased from Millipore Sigma (Burlington, MA, USA). All chemicals were of analytical grade and were used without further purification. Fish sperm DNA (74782) and Tris–HCl (RES3098T-B7) were supplied by Sigma-Aldrich Chemie GmbH (Germany). Ethidium bromide (EtBr) and sodium chloride (≥99.5%) were purchased from Sigma Aldrich, USA. Other chemicals and reagents purchased from Sigma or Merck and used in this work were all of the analytical grades.
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10

Solid-Phase Peptide Synthesis Protocol

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Dichloromethane (DCM), acetonitrile (ACN),
and HPLC grade water were supplied by Pharmco. 2-Chlorotrityl chloride
resin, dimethylformamide (DMF), bromoacetic acid, N,N-diisopropylethylamine (DIEA), diisopropylcarbodiimide
(DIC), trifluoroacetic acid (TFA), triisopropylsilane (TIPS), PyBOP,
benzylamine, 1-napthylmethylamine, and benzhydrylamine were provided
by Millipore Sigma. N-Boc-1,3-diaminopropane was
provided by Matrix Scientific.
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