Optical rotation was measured with a Horiba SEPA-300 polarimeter (Horiba, Kyoto, Japan). NMR spectra were recorded on Bruker DMX Avance 600 instruments equipped with an autotune probe and using the automation mode aided by the Bruker program. HREI-SMS spectra were determined on a micrOTOF-Q 98 spectrometer (Bruker-Daltonics, Bilerica, MA). For column chromatography, silica gel 60 particles size 0.04–0.063 mm (Merck, Darmstadt, Germany) and Sephadex LH-20 purchased at Sigma-Aldrich (St Louis, MO) were used. The plates were visualized using UV (254 and 366 nm) and revealed by spraying with vanillin-sulphuric acid (1% ethanolic solution of vanillin + 10% ethanolic sulphuric acid).
Avance dmx 600
Manufactured by Bruker
Sourced in Germany
The Avance DMX 600 is a high-performance nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It operates at a frequency of 600 MHz and is designed for high-resolution NMR applications in chemistry, materials science, and life sciences research.
Automatically generated - may contain errors
Lab products found in correlation
Sepa 300 polarimeter, by Horiba (2 mentions)
Sephadex lh 20, by Merck Group (2 mentions)
Uhr qtof maxis 4g, by Bruker (2 mentions)
P 2000 polarimeter, by Jasco (2 mentions)
Eurosphere 10 c18, by Knauer (1 mentions)
Eurosphere 100 c18, by Knauer (1 mentions)
Mn silica gel 60 m, by Merck Group (1 mentions)
Dimedone, by Merck Group (1 mentions)
Aromatic aldehydes, by Merck Group (1 mentions)
Histamine dihydrochloride, by Merck Group (1 mentions)
Jxa 8230, by JEOL (1 mentions)
Quantax 200, by Bruker (1 mentions)
Pw1730, by Philips (1 mentions)
8700 fourier transform spectrophotometer, by Shimadzu (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Eurospher 100 10 c18, by Knauer (1 mentions)
Ultimate 3000 system, by Thermo Fisher Scientific (1 mentions)
Silica gel 60 m, by Macherey-Nagel (1 mentions)
Silica gel 60 f254, by Macherey-Nagel (1 mentions)
Lc qdeca mass spectrometer, by Bruker (1 mentions)
7 protocols using avance dmx 600
1
Characterization of Chemical Compounds
2
Optical Rotation and Structural Characterization
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Horiba SEPA-300 polarimeter (HORIBA, Kyoto, Japan) was used to measure the optical rotation. NMR spectra were recorded on Bruker DMX Avance 600 instruments equipped with an autotune probe and using the automation mode aided by the Bruker program. HREI-SMS spectra were determined on a micrOTOF-Q 98 spectrometer. For column chromatography, silica gel 60 particle sizes 0.04–0.063 mm (Merck) and Sephadex LH-20 (Sigma) were used. The plates were visualized using UV (254 and 366 nm) and revealed by spraying with vanillin-sulphuric acid.
3
Circular Dichroism and NMR Analysis of Peptides
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CD was performed on a Jasco 1500 spectrometer using 1 mm-pathlength cells. Water and a solution of SDS 100 mM in water were used as solvents. Then, 16–32 scans were acquired at 25 °C between 190 and 280 nm. Peptide concentration: 0.1 mM. CD in fungi was performed on a sample prepared in 10 mM phosphate buffer at pH 7 incubated at 25 °C in the dark. Peptide final concentration: 50 µM. 2D NMR spectra were acquired at 313 K with a Bruker AVANCE DMX-600 instrument operating at a frequency of 600 MHz for 1H.
4
Spectroscopic Characterization of Organic Compounds
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A Jasco P-2000 polarimeter was used to measure the optical rotation. 1D and 2D NMR spectra were recorded on Bruker Avance DMX 600 or 700 NMR spectrometers. Chemical shifts were referenced to the solvent residual peaks. Mass spectra were recorded with a LC-MS HP1100 Agilent Finnigan LCQ Deca XP Thermoquest and HRESIMS were measured with a UHR-QTOF maXis 4G (Bruker Daltonics) mass spectrometer. HPLC analysis was performed on a Dionex 3000 RS system coupled with an Ultimate 3000 pump and a photodiode array detector (DAD 300RS). The analytical column (125 × 4 mm) was prefilled with Eurosphere-10 C18 (Knauer, Germany), and the following gradient solvent system was used: 0 min (10% MeOH), 5 min (10% MeOH), 35 min (100% MeOH), and 45 min (100% MeOH). Semi-preparative HPLC was performed using a Merck Hitachi HPLC System (UV detector L-7400; pump L-7100; Eurosphere-100 C18, 300 × 8 mm, Knauer) with MeOH–H2O as mobile phase and a flow rate of 5.0 mL min−1. Column chromatography was carried out using Merck MN silica gel 60 M (0.04–0.063 mm). TLC plates with silica gel F254 (Merck) were used to monitor and collect fractions under detection at 254 and 366 nm. Distilled and spectral-grade solvents were used for column chromatography and spectroscopic measurements, respectively.
5
Synthesis and Characterization of Nanomaterials
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Solvents and all materials were purchased from commercial resources and utilized as received without any further purification. Histamine dihydrochloride (Sigma-Aldrich, >99%), aromatic aldehydes (Merck, Fluka and Sigma-Aldrich, 98–99%), dimedone (Sigma-Aldrich, >97%), 4-hydroxycoumarin (Fluka, purum), and acetonitrile (Sigma-Aldrich, 99.8%) were used as received. The performed LEDs were commercial and no cutoff filter was used. Fourier transform infrared (FT-IR) spectra were recorded on a Shimadzu 8700 Fourier transform spectrophotometer in the range 400 to 4000 cm−1 with KBr pellets. UV-visible spectra were recorded on a Photonix UV-visible array spectrophotometer. X-ray diffraction (XRD) patterns were acquired on a PHILIPS PW 1730 diffractometer with Cu Kα at 30 mA, 40 keV and a scanning rate of 3° min−1 in the 2θ domain from 5 to 80°. Energy dispersive X-ray spectroscopy (EDS) was performed with an Electron Probe Microanalyser JEOL JXA-8230 equipped with an energy dispersive spectrometer Bruker QUANTAX 200. A Mira 3-MU field emission scanning electron microscope (FESEM) was used to investigate the morphology of the synthesized nanomaterials. Particle size and further morphology studies were performed on a TEM (Philips CM-200 and Titan Krios). NMR experiments were carried out on a Bruker Avance DMX600 instrument operating at 400 MHz for proton.
6
HPLC and Spectroscopic Analysis of Natural Compounds
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HPLC analysis was carried out with a Dionex UltiMate 3000 system coupled with an UltiMate 3000 pump linked to a photodiode array detector (DAD 3000 RS). Detection wavelengths were set at 235, 254, 280, and 340 nm. The column was prefilled with Eurospher 100-10 C18, 125 × 4 mm (Knauer, Germany). The routine HPLC analysis was performed with the following gradient (MeOH : 0.1% HCOOH in H2O): 0 min (10% MeOH); 5 min (10% MeOH); 35 min (100% MeOH); 45 min (100% MeOH). Semipreparative HPLC was conducted with a Merck Hitachi Chromaster HPLC system (UV detector 5410; pump 5110; column Eurospher 100-10 C18, 300 × 8 mm, Knauer; flow rate at 5 mL min−1). Silica gel 60 M (Macherey-Nagel) was used for vacuum liquid chromatography (VLC) and Sephadex LH-20 for column chromatography. TLC plates pre-coated with silica gel 60 F254 (Macherey-Nagel) were used for routine analysis. One- and two-dimensional NMR spectra were recorded on Bruker AVANCE DMX 600 or 500 NMR spectrometers. ESIMS and HRESIMS data were acquired by a Finnigan LCQ Deca mass spectrometer and an UHR-QTOF maXis 4G (Bruker Daltonics) mass spectrometer, respectively. FT-IR spectra were recorded on a Bruker Tensor 37 IR spectrometer in a range of 4000–400 cm−1 with the resolution of 4 cm−1 as a KBr pellet. Optical rotations were measured on a Jasco P-2000 polarimeter.
7
Analytical TLC, UV, NMR, and HPLC Analysis
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Analytical TLC: aluminum sheets silica gel Si 60 F254 (Merck, Darmstadt, Germany), detection by UV absorption at 254 nm and 366 nm, Dragendorff spray reagent (alkaloids) [13 (link)]. UV data were recorded on a Shimadzu UV/vis-2450 spectrophotometer using methanol (UVASOL, Merck, Darmstadt, Germany) as solvent. NMR spectra were recorded on Bruker Avance DMX 600 or Ascend DPX 500/700 (Bruker Biospin, Bremen, Germany) NMR spectrometers, locked to the deuterium signal of the solvent. Data acquisition, processing, and spectral analysis were performed with standard Bruker software and ACD/NMR workbook. Chemical shifts are given in parts per million (ppm), and coupling constants in hertz (Hz). HRESIMS data were recorded on a maXis ESI QTOF mass spectrometer (Bruker Daltonics, Bremen, Germany); molecular formulas were calculated using the isotopic pattern (Smart Formula algorithm). Analytical RP-HPLC was carried out with an Agilent 1260 system equipped with a diode-array UV detector and a Corona Ultra detector (Dionex, Germering, Germany). HPLC conditions: column 125 × 2 mm, Nucleodur C18, 5 μm (Macherey-Nagel, Düren, Germany), solvent A: 5% MeCN in water, 5 mmol NH4Ac, 0.04 mL/L AcOH; solvent B: 95% MeCN, 5 mmol NH4Ac, 0.04 mL/L AcOH; gradient system: 10% B increasing to 100% B in 30 min, 100% B for 10 min, to 10% B post-run for 10 min; 40 °C; flow rate 0.3 mL/min.
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