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8 protocols using molecular sieves 4

1

Comprehensive Phytochemical Profiling and Lipase Inhibition

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All plant samples were collected from Goesan-gun (Chungcheongbuk-do, Republic of Korea) in 2015 and were immediately cleaned, ground, lyophilized, and stored at −20 °C before use. Lipase from porcine pancreas type II, 4-methylumbelliferyl oleate (4-MUO), and quercetin (≥95%) was purchased from Sigma-Aldrich Co. (St. Louis, MO, USA). Kaempferol (≥98.3%), myricitrin (≥98.3%), quercitrin (≥98.5%), and avicularin (≥99.3%) were purchased from ChemFaces Biochemical Co. (Wuhan, Hubei, China), and their purity was confirmed analytically by proton nuclear magnetic resonance (1H-NMR) and HPLC. Methanol, n-hexane, and ethyl acetate (EtOAc) were purchased from Daejung Chemicals & Metals Co. (Siheung-si, Gyeonggi-do, Republic of Korea), and were of analytical grade. Water and acetonitrile purchased from J. T. Baker Co. (Phillipsburg, NJ, USA) were of high-performance liquid chromatography (HPLC) grade. The acetonitrile was dehydrated by molecular sieves 4 Å (Sigma-Aldrich Co.) and filtered through a membrane filter (0.45 µm) before use. All of the other chemicals were of extra-pure grade.
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2

Fabrication and Characterization of Lipid Bilayers

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A silicon wafer polished on both side was purchased from Silicon Valley Microelectronics, Inc. (Santa Clara, CA, USA), stock ampules (25 mg) of 1,2-dipalmitoyl-sn-glycero-3-phosphoethanolamine (DPPE) and 1,2-dipalmitoyl-sn-glycero-3-phosphoserine (DPPS) were purchased from Avanti Polar Lipids Inc., (Alabaster, AL, USA). Molecular sieves 4 Å and nylon filter (0.2 μm) were purchased from Sigma-Aldrich Corp. (St. Louis, MO, USA). Silicon Nitride cantilevers with spring constants 0.3 N/m were purchased from Bruker Inc. (Camarillo, CA, USA). The instruments used include a Branson 1510 sonicator bath, a white light interferometer (WYKO NT1100, Veeco, Tucson, AZ, USA, a surface profiler (TENCOR P10, KLA-Tencor, Milpitas, CA, USA), a Plasma-Therm 790 Series (Saint Petersburg, FL, USA), a scanning electron microscope (LEO1550, Pleasanton, CA, USA), an atomic force microscope (Pico Plus AFM 1550 from Molecular Imaging, Keysight Technologies, Santa Rosa, CA, USA), and an electrochemical impedance spectroscope (VersaSTAT MC by Princeton Applied Research, AMETEK, Berwyn, PA, USA.
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3

Extraction of Blackcurrant Polyphenols

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Blackcurrant pomace was obtained from GlaxoSmithKline, Brentford, UK and more recently from A&R House Ltd., Bleadon, UK. The raw fruit grown in the UK had been pressed in production of blackcurrant cordial (Ribena) (Lucozade Ribena Suntory Ltd, 2018) . The crude waste is referred to as pomace, which comprises the fruit skins (ca. 50% w/w), seeds (ca. 45% w/w) and extraneous matter (e.g., berry stalks, ca. 5% w/w). Seeds are separated from this pomace and unwanted stalks removed; the subsequent material received was predominantly dried blackcurrant fruit skins, used without any further modification. Amberlite XAD7HP was obtained from Rohm & Haas (Staines, UK).
Delphinidin-3-O-glucoside was purchased from Polyphenols AS, Sandnes, Norway. Reversed-phase C18 (RP-C18) silica gel (40 63 µm) LiChroprep was provided by Merck (Darmstadt, Germany). Fatty acids, lipase acrylic resin from Candida antarctica lipase B (≥ 5000 U/g, recombinant, expressed in Aspergillus niger), molecular sieves 4Å, 2-methyl-2-butanol, and other general purpose chemicals were obtained from Sigma-Aldrich (Madrid, Spain).
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4

Synthesis and Characterization of Thyroid Hormone Analogues

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All commercial reagents used were of analytical grade and were used without further purification. Triiodothyronine (T 3 ) and thyroxine (T 4 ), potassium hexacyanoferrate (III), potassium 4/20 hexacyanoferrate (II) trihydrate (the pair [Fe(CN) 6 ] 3-/4-), 4-aminobenzoic acid (4-ABA), hydrochloric acid, tert-butyl (4-hydroxyphenethyl)carbamate, (4-(methoxymethoxy)phenyl)boronic acid, copper (II) acetate, pyridine, epinephrine, norepinephrine, dopamine, triethylamine, trifluoroacetic acid and molecular sieves 4 Å were purchased from Sigma-Aldrich, methanol was purchased from Merck. Phosphate buffer solution (PBS), 0.1 mol L -1 , pH 7.4 was prepared with potassium dihydrogen phosphate (KH 2 PO 4 ) and potassium hydrogen phosphate (K 2 HPO 4 ), both from Riedel-de-Haën.
Ultrapure water (resistivity not less than 18.2 Ω cm at 298 K) from a Direct-Q 3UV water purification system (Millipore) was used in all experiments. Thin-layer chromatography (TLC) was carried out on precoated silica gel 60 F254 (Merck) with layer thickness of 0. following the synthetic strategies shown in Fig. 1.
The compounds were obtained in moderate to high yields and fully characterized by magnetic resonance spectroscopy ( 1 HRMN, 13 All RMN spectra are present in the Supporting Information.
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5

Enzymatic Biodiesel Production from Soybean Oil

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Analytical grade reagents were used to prepare all solutions. Sulfuric acid (98 wt%) was acquired from Vetec®, hydrochloric acid (37 wt%) were purchased from Dinâmica®; isopropyl alcohol (99.5 wt%), sodium periodate (99.8 wt%), monoethylene glycol (99 wt%), sodium hydroxide (>97 wt%) and potassium hydroxide (>97 wt%) were purchased from Neon. Absolute methanol (99.95 wt%), absolute ethanol (99.95 wt%), THF and ammonium hydroxide (99.8 wt%) were acquired from Merck®. lauric acid (99.8 wt%), Candida antarctica Lipase A (CAL-A) recombinant from Aspergillus oryzae, and 4 Å molecular sieves were purchased from Sigma-Aldrich®. Lipozyme 435 and lipozyme TLIM were purchased from Novozyme®, and Soya® soybean oil was acquired at local market.
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6

Fabrication of NCM811 and LFP Electrodes

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Active materials (LiNi0.8Co0.1Mn0.1O2 (NCM811) or LiFePO4 powders), Super C65, polyvinylidene fluoride (PVDF), anhydrous N-methyl-2-pyrrolidone (NMP), carbon-coated aluminum (Al, 15 μm-thick) foil and Al2O3-coated polyethene (PE, 16 μm thick, 43% porosity) were purchased from the Guangdong Canrd New Energy Technology Co., Ltd. 1,3,5-trioxane (TXE, >99.0% (GC)) and 2,2,2-trifluoro-N, N-dimethylacetamide (FDMA, >98.0% (GC)) were purchased from Tokyo Chemical Industry Co., Ltd. FEC (99.95%), DMC (99.95%), LiDFOB (99.9%) and the reference carbonate electrolyte (i.e., 1M LiPF6 in EC:DMC 1;1 v/v non-aqueous liquid electrolyte solution) were purchased from DoDoChem. Li foils (50 or 250 μm) were purchased from China Energy Lithium Co., Ltd. FDMA was dried with 4 Å molecular sieves (Sigma–Aldrich) before use.
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7

Synthesis and Characterization of Fluorescent Probe

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All reagents for compound synthesis were used as supplied, and all solvents were ACS grade or better. Anhydrous solvents were stored over activated 4Å molecular sieves (Sigma Aldrich, 208604–1KG). The starting material 6-OH-BTA-1 (PiB) was obtained from ABX Biochemicals (Radeberg, Germany). The reagents propargyl-PEG3-bromide (BP-22738) and 5/6-carboxyrhodamine 110-PEG3-azide (BP-22478) were obtained from BroadPharm Inc. (San Diego, California).
Silica gel (pore size 60 Å, 200–400 mesh particle size) for column chromatography was obtained from Sigma Aldrich (Sigma Aldrich, 288549–500G). Analytical thin-layer chromatography was performed using glass-backed silica gel 60 F254 TLC plates (Millipore, 1057150001) and aluminum-backed C18-W (RP-18W) silica F254 TLC plates (Sorbtech, 2733167). Preparative thin-layer chromatography (pTLC) was performed using glass-backed C18-W (RP-18W) silica F254 pTLC plates (Sorbtech, 2717124). Before use, pTLC plates were pre-washed with an overnight immersion in methanol followed by developing twice in methanol. The pTLC plates were then air-dried and activated at 120 ™C for 2 hours, after which they were stored in a desiccator until use. All 96-well plate-based fluorescence intensity measurements were recorded using a Biotek Synergy 4 plate reader (BioTek Instruments) using the xenon flash bulb.
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8

Synthesis of V2O5 Thin Films

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Four types of precursor solutions were prepared to produce V2O5 thin films where the dilution of the alkoxide to the solvent and also the effect of two different types of additives to the precursor could be studied. Vanadium (V) oxytriisopropoxide OV(OCH(CH3)2)3 and PEG-400 was purchased from Sigma-Aldrich, and isopropyl alcohol (IPA) was used as-received.
For preparing the low and high dilution precursors, the IPA was mixed by volume with the vanadium oxytriisopropoxide precursor and the chosen additive at a volume ratio of 1000:10:1 and 250:10:1 (IPA : Alkoxide : Additive) respectively. Deionized water was added as an additive to the precursor solution to aid the hydrolysis and was replaced by the same liquid volume of PEG-400 in the polymer-assisted deposition (PAD) precursor solutions. The prepared solutions were stored in closed vials with 4 Å molecular sieves from Sigma-Aldrich to increase their shelf life by preventing hydrolysis from the environment prior to the deposition. As mentioned in the main text, four types of precursor solution were prepared: a low concentration dilution (LCP) and high concentration dilution (HCP) solution where the additive was deionized H2O, the precursor solutions prepared using PEG-400 as an additive were a low (LCP-PEG) and high (HCP-PEG) dilution mixture.
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