Elemental analyses were carried out with a PerkinElmer 2400-II or were performed by the Institute of Chemical and Physical Research Analytical Facility, Wako Saitama, Japan. FAB MS spectra were measured with a JEOL JMS-700 spectrometer with m-nitrobenzyl alcohol using as matrix. 1H and 13C NMR spectra were obtained with a JEOL JML-AL300 and AL500 spectrometers. UV-vis spectra were measured on a Shimadzu MultiSpec-1500 or UV-3600 Plus. IR spectra were recorded on a Shimadzu IR Affinity-1 spectrophotometer using samples prepared as KBr disks. Electrochemical measurements were made in CH3NO2 solutions containing 0.1 mol dm−3 tetra-n-buthylammonium perchlorate (TBAP, Nakarai Tesque Ltd.) as a supporting electrolyte and an Ag|0.01 mol dm−3 AgNO3 reference or in H2O–DMSO (2 : 3 (v/v)) solutions containing 0.2 M HClO4–NaOH aqueous solution with a glassy carbon working electrode (ϕ = 1.6 mm), an Ag|AgCl 3.0 M NaCl reference electrode, and a platinum wire counter electrode using an ALS 630E electrochemical analyzer. At the end of each measurement, ferrocene (Fc) was added as an internal standard to correct redox potentials (E(Fc+/Fc) = 0.074 V vs. Ag|0.01 mol dm−3 AgNO3). Caution! Perchloric acid is potentially explosive and should be handled with care.
Jms 700 spectrometer
Manufactured by JEOL
Sourced in Japan
The JMS-700 spectrometer is a high-performance mass spectrometry instrument manufactured by JEOL. It is designed to provide accurate and reliable mass analysis of a wide range of chemical compounds. The JMS-700 utilizes advanced ionization techniques and a powerful mass analyzer to deliver precise mass measurements and detailed structural information. Its core function is to enable researchers and analysts to accurately identify and characterize various molecules and substances.
Automatically generated - may contain errors
Lab products found in correlation
Ez melt mpa120, by Stanford Research Systems (6 mentions)
Av 400 nmr spectrometer, by Bruker (3 mentions)
Silica gel 60 f254 plate, by Merck Group (3 mentions)
Wakogel c 200, by Fujifilm (2 mentions)
13c nmr 150 mhz, by Agilent Technologies (2 mentions)
Ft ir 4100 spectrometer, by Jasco (2 mentions)
Kieselgel 60 f254 plate, by Merck Group (2 mentions)
F254 merck plates, by Merck Group (2 mentions)
Oxford 600 mhz spectrometer, by Agilent Technologies (2 mentions)
Silica gel 60n, by Kanto Chemical (2 mentions)
Ft ir nicolet is5 spectrometer, by Thermo Fisher Scientific (2 mentions)
Ods silica gel gel ods a, by YMC (2 mentions)
Thioflavin t, by Fujifilm (2 mentions)
Synergy htx multi mode reader, by Agilent Technologies (2 mentions)
Avance 3 400 mhz, by Bruker (2 mentions)
P 2000 digital polarimeter, by Jasco (2 mentions)
Dimethyl sulfoxide (dmso), by Fujifilm (2 mentions)
Multispec 1500, by Shimadzu (1 mentions)
Uv 3600 plus, by Shimadzu (1 mentions)
Iraffinity 1 spectrophotometer, by Shimadzu (1 mentions)
41 protocols using jms 700 spectrometer
1
Instrumental Characterization of Compounds
2
Spectroscopic Analysis of Organic Compounds
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All of the reagents that we used are commercially available and were purchased from Sigma Aldrich® (Saint Louis, MO, USA) or Merck® (Darmstadt, Germany). 1H and 13C nuclear magnetic resonance spectra were obtained on a Variant Oxford Instrument (Palo Alto, CA, USA, 600 MHz and 150 MHz, respectively). DMSO-d6 was used as a deuterated solvent. Molecular masses were obtained with a JMS-700 spectrometer (JEOL, Tokyo, Japan) with an impact electronic method (70 eV). Melting points were obtained using an EZ-Melt MPA120 automated apparatus from Stanford Research Systems (Sunnyvale, CA, USA). Thin layer chromatography (TLC) was conducted on silica gel plates (Merck, Darmstadt, Germany).
3
Isolation of Anti-Inflammatory Compounds from E. amstelodami
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According to the results of MTT and NO production assays, the strain, E. amstelodami (015-2) was selected as the target strain for the isolation of nature products and evaluation of their anti-inflammatory activity. The fugal strain was cultured (8 L) for 30 d (static) at 29 °C in SWS medium containing of soytone (0.1%), soluble starch (1.0%) and seawater (100%). The BE were prepared according to the above methods (015-2B) (0.7 g). The BE (0.7 g) which showed higher inhibitory effect against NO production was subjected to silica gel flash chromatography (n-hexane/EtOAc, EtOAc/MeOH) to furnish twelve fractions (Fr. B1-B12) on the basis of TLC analysis. Fr. B7 (161.2 mg) was further purified by Sephadex LH-20 column eluting with MeOH to give crude compound 1 and compound 2 . Final purification of each crude compound by HPLC (Sunfire, Waters, 50% MeOH) yielded the compound 1 (25.2 mg) and 2 (35.6 mg). Fr. B10 (130.5 mg) was further purified by Sephadex LH-20 column eluting with MeOH to give crude compound 3 . Then, the fraction was finally purified by ODS column to afford compound 3 (4.6 mg).
The 1H-NMR and 13C-NMR spectra of the isolated compounds were recorded on a JEOL JNM-ECP 400 MHz NMR spectrometer, using DMSO-d6 solvent peak (2.50 ppm in 1H and 39.5 ppm in 13C-NMR) as an internal reference standard. MS spectra were obtained on a JEOL JMS-700 spectrometer.
The 1H-NMR and 13C-NMR spectra of the isolated compounds were recorded on a JEOL JNM-ECP 400 MHz NMR spectrometer, using DMSO-d6 solvent peak (2.50 ppm in 1H and 39.5 ppm in 13C-NMR) as an internal reference standard. MS spectra were obtained on a JEOL JMS-700 spectrometer.
4
Structural Characterization of Biomolecules
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The LC-MS/MS analyses were performed using an LC-MS system (Waters, Milford, MA, USA) consisting of an Acquity ultra-performance liquid chromatograph and an Acquity quadruple tandem mass spectrometer (TQ Detector). The data acquisition and analyses were performed using MassLynx v. 4.1 software (Waters). NMR, circular dichroism (CD), and electron ionization MS spectra were recorded on a JMN-AL 300 spectrometer (JEOL, Tokyo, Japan), J-805 spectropolarimeter (JASCO, Tokyo, Japan), and JMS-700 spectrometer (JEOL), respectively.
5
Analytical Characterization of Organic Compounds
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All reagents and solvents
were purchased from commercial suppliers and used without further
purification. IR spectra were recorded with an IR Affinity-1S spectrophotometer
(ATR, Shimazu Corp. Kyoto, Japan). 1D and 2D NMR spectra were measured
at 298 K with a Varian 400 MR (400 MHz) spectrometer (Agilent Technologies
Japan, Ltd., Tokyo, Japan) and a Bruker Avance NEO 400 MHz spectrometer
(Bruker Japan K.K., Kanagawa, Japan) using tetramethylsilane as the
internal standard. Low- and high-resolution EI and FABMS spectra were
measured with a JMS-700 spectrometer (JEOL, Tokyo, Japan). Column
chromatography was performed using Wakogel C-200 (FUJIFILM Wako Pure
Chemical Corporation, Osaka, Japan). Analytical and preparative HPLC
was performed on a Jasco PU-4580 equipped with a Jasco UV-4570 detector
(Jasco Corp., Tokyo, Japan) at 254 nm. Preparative HPLC columns were
Inertsil diol columns (ϕ10 × 250 mm, 5 μm, GL Sciences
Inc., Tokyo, Japan).
were purchased from commercial suppliers and used without further
purification. IR spectra were recorded with an IR Affinity-1S spectrophotometer
(ATR, Shimazu Corp. Kyoto, Japan). 1D and 2D NMR spectra were measured
at 298 K with a Varian 400 MR (400 MHz) spectrometer (Agilent Technologies
Japan, Ltd., Tokyo, Japan) and a Bruker Avance NEO 400 MHz spectrometer
(Bruker Japan K.K., Kanagawa, Japan) using tetramethylsilane as the
internal standard. Low- and high-resolution EI and FABMS spectra were
measured with a JMS-700 spectrometer (JEOL, Tokyo, Japan). Column
chromatography was performed using Wakogel C-200 (FUJIFILM Wako Pure
Chemical Corporation, Osaka, Japan). Analytical and preparative HPLC
was performed on a Jasco PU-4580 equipped with a Jasco UV-4570 detector
(Jasco Corp., Tokyo, Japan) at 254 nm. Preparative HPLC columns were
Inertsil diol columns (ϕ10 × 250 mm, 5 μm, GL Sciences
Inc., Tokyo, Japan).
6
Spectroscopic Analysis of Organic Compounds
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Melting points were determined in an A9200 digital melting point instrument from Thermo Scientific; the results are uncorrected. All reactions were monitored by thin-layer chromatography (TLC) and carried out using glass plates precoated with silica gel 60 F254 (Merck, Kenilworth, NJ, USA). 1H NMR spectra were determined on Varian 600 MHz AR Premium Compact and 13C NMR (150 MHz) instruments (Varian-Agilent, Santa Clara, CA, USA). Chemical shifts are reported in ppm DMSO-d6 and CDCl3 as deuterated solvents. Mass spectrometry was obtained from a JEOL JMS-700 spectrometer by electronic impact (JEOL, Tokyo, Japan).
7
Moisture- and Air-Sensitive Organic Synthesis
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All experiments with moisture- and air-sensitive compounds were performed in anhydrous solvents under nitrogen atmosphere in flame-dried glassware. All reagents were purchased from commercial sources and used without further purification unless otherwise noted. The microwave experiment was carried out with a Biotage Initiator Eight EXP. UV–vis absorption spectra were recorded on a JASCO V-670 spectrometer and a SHIMADZU UV-1800 spectrometer. Fluorescence spectra were recorded on a JASCO FP-6500 spectrometer. Melting points were determined on a Stanford Research Systems MPA 100 or a Yanako MP-500P apparatus and were uncorrected. Infrared (IR) spectra were recorded on a JASCO FT IR-4100 spectrometer using dispersed KBr pellets. 1H and 13C NMR spectra were measured at 23 °C on a JEOL RESONANCE JNM-ECZ400S spectrometer at 400 MHz and 100 MHz, respectively. CDCl3 was used as a solvent and the residual solvent peaks were used as an internal standard (1H NMR: CDCl3 7.26 ppm; 13C NMR: CDCl3 77.00 ppm). High-resolution fast atom bombardment (FAB) mass spectra were measured on a JEOL JMS-700 spectrometer. TLC analysis was performed using Merck silica gel 60 F254, and the preparative TLC (PTLC) purification was conducted using Wakogel B-5F PTLC plates. Elemental analyses were measured on a J-Science Micro corder JM10 at the Analysis Center at Osaka University.
8
Synthesis and Evaluation of Polyamine Inhibitors
9
Characterization of Organophosphorus Compounds
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All solution‐phase reactions were conducted under an argon atmosphere. 1H NMR spectra were obtained at 300 MHz on a JEOL Al300 spectrometer and at 400 MHz on a JEOL Lambda 400 spectrometer with tetramethylsilane (TMS) as an internal standard (δ 0.0) in CDCl3. 31P NMR spectra were obtained at 162.0 MHz on a JEOL Lambda 400 spectrometer with 85 % H3PO4 (δ 0.0) as an external standard. 19F NMR spectra were obtained at 376.3 MHz on a JEOL Lambda 400 spectrometer. Mass spectra were recorded on a JMS‐700 spectrometer (JEOL) with trifluoroacetic acid as an external standard (δ−76.5). Mass spectra were recorded on a 910‐MS FTMS system (Varian) or a Voyager System 4327 (Applied Biosystems). Analytical TLC was performed on Merck Kieselgel 60‐F254 plates. Silica gel column chromatography was carried out using silica gel 60 n (63–210 μm or 40–50 μm) as a neutral silica gel, and Chromatorex NH‐DM1020 as an NH silica gel. Gel filtration chromatography was conducted using Sephadex® LH‐20. RP‐HPLC was carried out using a μBondasphere 5 μm C18, 100 Å, 3.9 mm × 150 mm (Waters). Organic solvents were purified and dried according to the appropriate procedures. Anomeric ratio was calculated from relative peak areas in 19F NMR and 31P NMR.
10
Spectroscopic Characterization of Organic Compound
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Melting point was determined by a Fisher Scientific melting point measuring apparatus without corrections. The IR spectrum was obtained, as a KBr disc, on a Bruker Tensor 27 FT-IR spectrometer. Optical rotation was measured with an Atago AP-300 automatic polarimeter. 1H- and 13C-NMR, COSY, HMQC, HMBC, and NOESY spectra were recorded on the Varian Unity 400 and Bruker AV 500 NMR spectrometers, using tetramethylsilane (TMS) as the internal standard. Standard pulse sequences and parameters were used for the NMR experiments and all chemical shifts were reported in parts per million (ppm, δ). The low and high-resolution FAB mass spectra were obtained on a JEOL JMS-700 spectrometer operated in the positive-ion mode. All the chemicals were purchased from Merck KGaA (Darmstadt, Germany) unless specifically indicated. Column chromatography was performed on silica gels (Kieselgel 60, 70–230 mesh, Merck KGaA). Thin layer chromatography (TLC) was conducted on precoated Kieselgel 60 F 254 plates (Merck) and the compounds were visualized by UV light or spraying with 10% (v/v) H2SO4 followed by heating at 110°C for 10 min.
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