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14 protocols using v 660 spectrometer

1

Spectroscopic and Thermal Analysis of Coordination Compounds

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The UV-Vis diffuse reflectance spectra were recorded on a Jasco V-660 spectrometer (Jasco, Easton, MD, USA), in the spectral range 200–850 nm, using spectralon [56 (link)] as a standard with 100% reflectance. The three-dimensional fluorescence spectra were recorded on a Jasco FP-6300 spectrofluorometer (Jasco, Easton, MD, USA), with solid samples directed at an angle of 30° to the incident beam. The excitation and emission wavelength ranges were 220–640 nm and 230–740 nm, respectively. The data pitch and bandwidth were 1 nm on both monochromators. The ATR-IR spectra of the coordination compounds were recorded on a Bruker INVENIO-R spectrometer (Bruker Optik GmbH, Ettlingen, Germany) in the spectral range 4000–400 cm−1. The thermal analyses were carried out with a Netzsch STA 449 F1 Jupiter thermoanalyzer (Netzsch-Geratebau GmbH, Selb, Germany) coupled with a Netzsch Aeolos Quadro QMS 403 mass spectrometer (Netzsch-Geratebau GmbH, Selb, Germany). Samples were heated in corundum crucibles up to 1000 °C, with a heating rate 10 °C∙min−1 in synthetic air (20% O2, 80% N2) flow.
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2

Physicochemical Characterization of Azo Compounds

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NMR spectra were recorded on Bruker Avance III 500 (1H: 500 MHz, 13C: 125 MHz) and Bruker Avance III HD 600 MHz (1H: 600 MHz, 13C: 150 MHz) NMR instruments (Bruker Biospin, Ettlingen, Germany). Melting points were determined in open capillary tubes using a STUART SMP3 electric melting point apparatus (Bibby Sterilin Ltd., Stone, UK) and are uncorrected. Elemental analysis was performed with a multi EA 4000 (Analytik Jena, Jena, Germany) device.
Absorption spectra of all azo derivatives were recorded using a Jasco V-660 spectrometer (Jasco Corporation, Tokyo, Japan) in the 200–800 nm range, at room temperature, in a 1 cm quartz cuvette.
Fluorescence emission of the azo derivatives was measured on powder, using a OceanInsight XDH spectrometer (OceanInsight, Orlando, FL, USA) modular device coupled via optical fiber to a LED source emitting at 365 nm on reflection mode, and in solution using a Jasco V850 spectro-fluorimeter (Jasco Corporation, Tokyo, Japan). FTIR spectra were collected using a Tensor 37 Bruker equipment (Bruker Corporation, Billerica, MA, USA) instrument within the spectral range 400–4000 cm−1, with 32 scans at a resolution of 4 cm−1. Sample pellets were prepared by adding azo dye powder to KBr powder.
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3

Characterization of Novel Materials via Spectroscopic Techniques

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The FT-IR spectra were recorded on the Jasco FT/IR 6200 spectrophotometer (JASCO, Easton, MD, USA), in the form of KBr pellets, in the spectral range 4000–400 cm−1. The UV-Vis diffuse reflectance spectra were recorded on a Jasco V-660 spectrometer (Jasco, Easton, MD, USA), in the spectral range 190–800 nm, using spectralon [44 (link)] as a standard with 100% reflectance. The thermal decompositions were carried out with the Netzsch STA 449 F1 Jupiter thermoanalyzer (Netzsch-Geratebau GmbH, Selb, Germany) coupled with the Netzsch Aeolos Quadro QMS 403 mass spectrometer (Netzsch-Geratebau GmbH, Selb, Germany). Samples were heated in corundum crucibles, in the temperature range 35–1000 °C, with the heating rate of 10 °C/min in synthetic air (80% N2, 20% O2). The XRPD patterns were recorded in a reflection mode on the XPert PRO MPD diffractometer (Malvern Panalytical Ltd., Royston, UK) equipped with CuKα1 radiation, a Bragg–Brentano PW 3050/65 high-resolution goniometer, and PW 3011/20 proportional point detector.
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4

Brain Tissue Clearing and Optical Density

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All animals were handled in accordance with the Japanese national guidelines for the care and use of laboratory animals and with the approval of the Animal Care and Use Committee of the Tokyo University of Science. Brain samples isolated from adult ICR mice sacrificed under hyper-anesthesia were minced by using a BioMasher (Nippi Inc., Tokyo, Japan), suspended in PBS, and fixed using 4 wt% formaldehyde in PBS overnight. Fixed cell suspension was collected by centrifugation (1200 × g, 5 min), washed with PBS three times, and divided into different tubes. The cell suspensions were then incubated in either ScaleA2, PBS, or an aqueous solution of urea (4 M), indium chloride (4 M), sodium iodide (2, 4 M), Triton X-100 (10 wt%), phosphoric acid (8.5, 11.4, 14.2 M), or 0.1 wt% Triton X-100 in phosphoric acid (14.2 M) for 24 h at room temperature. The OD600 was measured by means of a V-660 spectrometer (JASCO) and a 1.5 mL disposable cuvette (Brand GmbH & Co. KG, Wertheim, Germany).
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5

Spectroscopic Analysis of CraCRY Variants

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Absorption spectra of CraCRY variants were recorded using a V-660 spectrometer (JASCO). The protein solutions were measured in a low salt buffer (10 mM Tris, 100 mM sodium chloride, pH 7.8) with varying concentrations of dithiothreitol (DTT) and tris(2-carboxyethyl)phosphine (TCEP). Spectra were recorded after different illumination times using a high power LED (λmax = 450 nm; 9.7 mW cm−2 at a distance of 10 cm, Roithner Lasertechnik) at 2 °C. To simulate a HDX-MS measurement samples were put in the light chamber, which was cooled at 4 °C.
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6

Spectroscopic Analysis of CraCRY Variants

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Absorption spectra of CraCRY variants were recorded using a V-660 spectrometer (JASCO). The protein solutions were measured in buffer containing 50 mM NaH2PO4 pH 7.8, 100 mM NaCl and 20% (v/v) glycerol. The samples were incubated for 5 min in the dark before first spectra were recorded. Spectra were measured after different illumination times using a high power LED 450 nm (9.7 mW cm−2 at a distance of 10 cm, Roithner Lasertechnik) at 10°C.
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7

Chloroform Solvent Purification and Characterization

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All chemicals and
solvents were of commercial reagent quality and used without further
purification unless otherwise stated. CHCl3 (Kanto, extra
pure) stabilized with 0.5–1% ethanol was used. UV–vis
absorption spectra were collected on a JASCO V-660 spectrometer at
298 K.
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8

Liposome Preparation and Optical Characterization

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Liposome suspension was prepared by the Bangham method.31 (link) Briefly, a mixture of 12 μmol of DPPC, 12 μmol of DOPC, 12 μmol of cholesterol, and 4 μmol of DSPE-PEG was prepared in 1600 μL of chloroform in an eggplant-shaped glass flask, and then evaporated at 37 °C to remove chloroform and to obtain a thin lipid bilayer on the inner wall of the flask. 7.5 mL of either distilled water, aqueous solution of urea (4 M) or phosphoric acid (14.2 M) was added into the flask and sonicated to prepare a liposome suspension in each liquid. The optical loss (OD600) of the liposome suspensions was measured by using a V-660 spectrometer (JASCO Co., Tokyo, Japan) and a 1.5 mL disposable cuvette (Brand GmbH & Co. KG, Wertheim, Germany).
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9

Photostability of Curcumin in Pluronic Micelles

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Absorption and fluorescence spectra of Curcumin solubilized in Pluronic micelles and in various model solvents were recorded. Curcumin was dissolved in ethanol, DMSO, acetonitrile, and 1.5% (w/v) Pluronic solutions in PBS to obtain solutions with the final concentration of 0.005 mg/mL. The measurements were carried out by using a Jasco V-660 spectrometer (Jasco Corporation, Tokyo, Japan) and a Jasco FP6300 spectrofluorimeter (Jasco Corporation, Tokyo, Japan).
The photostability of the drug encapsulated in micelles was investigated using changes in fluorescence emissions after exposure to blue light. Curcumin in different Pluronic micellar solutions (0.2 μg/mL) were prepared as described earlier. Samples were placed in a quartz cuvette (1 cm optical pathway) and excited at 470 nm using the optical system of the above-mentioned spectrofluorimeter for 5, 15, 30, and 45 min, and the fluorescence spectra were recorded. The amount of undecayed CURC was calculated using the equation: Undecayed Curcumin%=Amount of Curcumin DeterminedAmount of Curcumin Used×100
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10

Synthesis and Characterization of Air-Sensitive Compounds

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All reactions treating air-sensitive compounds were performed under argon or nitrogen atmosphere using a high-vacuum line, standard Schlenk techniques, or a glove box, as well as dry and oxygen-free solvents. 1H (500 MHz), 11B (160 MHz), 13C (125 MHz), and 29Si (99 MHz) NMR spectra were recorded on a Bruker Avance III 500 FT NMR spectrometer. The 1H NMR chemical shifts in benzene-d6 (C6D6) were referenced to the residual C6D5H signal (δ 7.16). The 13C{1H} and 29Si{1H} NMR chemical shifts were relative to Me4Si (δ 0.00). The 11B NMR chemical shifts were relative to BF3·OEt2 (δ 0.00). Sampling of air-sensitive compounds was carried out using a VAC NEXUS 100027-type glove box. Mass spectra were recorded on a Bruker Daltonics SolariX 9.4T or a JEOL JMS-Q1050 spectrometer. UV-vis spectra were recorded on a JASCO V-660 spectrometer.
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