Optical rotations were measured on a JASCO DIP-1000 (JASCO Co., Ltd., Tokyo, Japan). Electrospray ionization-mass spectrometry spectra were obtained using a JEOL JMS-600W spectrometer (JEOL Ltd., Tokyo, Japan) (Supplementary Fig S3 ). NMR spectra were obtained using a Bruker AVANCE-400 (400.13 MHz for 1H) spectrometer (Bruker Bio Spin K. K., Kanagawa, Japan). The multiplicity of the signals was abbreviated as follows: s = singlet, d = doublet, dd = doublet of doublets, dt = doublet of triplets, t = triplet, q = quartet, m = multiplet, and br = broad. Column chromatography was conducted using sephadex LH-20 resin (GE healthcare Japan Co., Ltd., Tokyo, Japan). Thin-layer chromatography (silica gel, Merck Ltd., Japan) was conducted using van Urk reagent (Ehmann, 1977 ). Preparative high-performance liquid chromatography (HPLC) was conducted using an LC-20AT prominence pump (flow rate 2 mL min-1, Shimadzu Corp., Kyoto, Japan) and an Inertsil ODS-P column (10 × 250 mm, GL science Inc., Tokyo, Japan) in a CO-965 column oven (30 °C, JASCO Co., Ltd., Tokyo, Japan,) and monitored with an SPD-20A UV detector (Shimadzu Corp., Kyoto, Japan). A BioShaker PERSONAL-11 (TAITEC Co., Ltd., Saitama, Japan) was used for the incubation of A. take.
Jms 600w spectrometer
Manufactured by JEOL
Sourced in Japan
The JMS-600W spectrometer is a scientific instrument designed for mass spectrometry analysis. It is capable of precisely measuring the mass-to-charge ratios of various molecules and ions within a sample. The core function of the JMS-600W is to provide accurate and reliable data for researchers and scientists working in fields such as chemistry, biology, and materials science.
Automatically generated - may contain errors
Lab products found in correlation
Dip 1000, by Jasco (2 mentions)
Sephadex lh 20 resin, by GE Healthcare (1 mentions)
Co 965 column oven, by Jasco (1 mentions)
Silica gel, by Merck Group (1 mentions)
Spd 20a uv detector, by Shimadzu (1 mentions)
Avance 400, by Bruker (1 mentions)
Ft ir 4100 spectrometer, by Jasco (1 mentions)
1260 quadrupole, by Waters Corporation (1 mentions)
Avance 700 spectrometer, by Bruker (1 mentions)
Micromass zq lc ms system, by Phenomenex (1 mentions)
B 540, by Büchi (1 mentions)
640 ir spectrometer, by Agilent Technologies (1 mentions)
Kieselgel 60, by Merck Group (1 mentions)
Rotary evaporator, by Büchi (1 mentions)
1260 infinity system, by Agilent Technologies (1 mentions)
Avance 500 nmr spectrometer, by Bruker (1 mentions)
5 protocols using jms 600w spectrometer
1
Analytical Techniques for Spectroscopic Characterization
2
Spectroscopic Characterization of Compounds
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Melting points were measured on a Yanagimoto micro-melting point apparatus (Yanaco New Science Inc., Kyoto, Japan). Optical rotations were measured on a JASCO DIP-1000 (JASCO Co., Ltd., Tokyo, Japan). CD spectra were obtained with a JASCO J-820 spectrophotometer (JASCO Co., Ltd.). UV spectra were recorded on an Amersham Biosciences, Ultrospec 2100 spectropolarimeter (GE Healthcare Japan Corp., Tokyo, Japan). Measurements of IR spectra were performed with a JASCO FT/IR-4100 spectrometer on a KBr cell (JASCO Co., Ltd.). NMR spectra (both 1 and 2D) were obtained on a Bruker AVANCE-400 (400.13 MHz for 1 H and 100.61 MHz for 13 C) spectrometer (Bruker Bio Spin K. K., Kanagawa, Japan). Multiplicity of signals is abbreviated as follows: s, singlet; d, doublet; dd, doublet of doublet; dt, doublet of triplets; t, triplet; q, quartet; m, multiplet; br, broad. EI and CI-MS spectra were obtained from a JEOL JMS-600W spectrometer (JEOL Ltd., Tokyo, Japan). ESI-MS spectra were obtained from a JEOL T100LP spectrometer (JEOL Ltd.).
3
Analytical Methods for Chemical Characterization
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The optical rotation was measured using the Autopol III polarimeter with a 5 cm cell. Ultraviolet (UV) spectra were recorded on the Scinco UVS-2100 spectrophotometer and infrared (IR) spectra were recorded on the Scimitar 800 FT-IR spectrometer. Nuclear magnetic resonance (NMR) spectra were obtained using the Bruker Avance 700 spectrometer. Methanol (MeOH; δH 3.31, δC 49.3) resonances were used as internal references. High resolution fast atom bombardment mass spectroscopy (HRFABMS) was performed using the JEOL JMS-600W spectrometer (JEOL Ltd. Tokyo, Japan). Low-resolution LC/MS measurements were performed using the Agilent Technologies 1260 quadrupole and Waters Micromass ZQ LC/MS system using a reversed-phase column (Phenomenex Luna C18 (2) 100 Å, 50 mm × 4.6 mm, 5 µm) at a flow rate of 1.0 mL/min at the National Research Facilities and Equipment Center (NanoBioEnergy Materials Center) at Ewha Womans University. Column chromatography separation was performed using a C18 column via eluting with a gradient of MeOH and water (H2O). The fractions were purified using the Waters 1525 binary high-performance liquid chromatography (HPLC) pump with a reversed-phase C18 column (Phenomenex Luna C18 (2), 250 mm × 10 mm, 5 μm) via eluting with 30% acetonitrile (CH3CN) in H2O at flow rate of 2.0 mL/min.
4
Synthesis and Characterization of Melatonin Derivatives
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All reagents from commercial sources were used as sold, without further purification. Organic solvents were concentrated under reduced pressure using a Büchi rotary evaporator. Thin‐layer chromatography (TLC) analyses were performed using Merck precoated TLC plates (silica gel 60 GF254, 0.25 mm). Flash column chromatography was carried out using E. Merck Kieselgel 60 (70‐230 mesh). Melting points were recorded on a Büchi B‐540 melting‐point apparatus. High‐resolution mass spectra (HRMS) were measured on a JEOL JMS‐600W spectrometer. Nuclear magnetic resonance (1H‐NMR and 13C‐NMR) spectra were measured on a VNMRS‐500 [500 MHz (1H), 125 MHz (13C)] spectrometer, using CHCl3‐d as the solvent, and were reported in ppm relative to CHCl3 (δ 7.24) for 1H‐NMR and relative to the central CDCl3 resonance for 13C‐NMR. Coupling constants (J) in 1H‐NMR are in Hz. Fourier‐transform infrared spectra (FT‐IR) were measured on a VARIAN 640‐IR spectrometer. Log P (P: partition coefficient for n‐octanol/water) was determined using ChemBioDraw Ultra software (v14.0) (PerkinElmer, MA, USA). The detailed synthetic procedures and characterizations of melatonin and its derivatives are described in the [Link] , [Link] .
5
Analytical Characterization of Compounds
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Medium-pressure liquid chromatography (MPLC) and HPLC were performed using the Buchi Sepacore Flash system (Flawil, Switzerland) consisting of a UV photometer C-640 and Agilent 1260 Infinity system (Tokyo, Japan) equipped with a diode array detector (DAD). Mass spectrometry (MS) was conducted using a JEOL JMS-600-W Spectrometer (Tokyo, Japan), and nuclear magnetic resonance (NMR) spectra were recorded using a Bruker AVANCE 500 NMR spectrometer (Rheinstetten, Germany) in CDCl 3 with tetramethylsilane used as the internal standard. Chemical shifts are reported in parts per million (δ) and the coupling constant (J) is expressed in Hertz (Hz). All reagents used were of analytical grade.
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