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Ascend 400 mhz nmr

Manufactured by Bruker

The Ascend 400 MHz NMR is a nuclear magnetic resonance spectrometer designed to provide high-resolution analyses of chemical compounds. It operates at a frequency of 400 MHz and is capable of performing various NMR experiments to determine the structural and chemical properties of samples.

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3 protocols using ascend 400 mhz nmr

1

Spectroscopic Verification of Dopamine Acrylate

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We used the hydrogen spectrum to verify whether dopamine acrylate (DAA) had been successfully synthesized. We weighed 0.038 g of DAA and dissolved it in 0.5 mL DMSO-d6, then added a dropper into the NMR test tube and used a Bruker Ascend 400 MHz NMR to detect the spectrum of dopamine acrylate.
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2

Isolation and Characterization of Deoxyrhapontigenin

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The crude extracts were sequentially fractionated with dichloromethane, ethyl acetate and followed by aqueous solvents. When the dichloromethane fraction was concentrated to dryness, the yield was 288.83 g. Around 60 g of crude extract from dichloromethane fraction was subjected to column chromatography using silica gel column. The column was eluted in sequence by increasing the percentage of ethyl acetate from 25% to 100% with hexane to give D1, D2, D3, and D4 fractions. The D2 fraction was concentrated (24.16 g), eluted in sequence by increasing the ratio of methanol from 2 to 100 with dichloromethane. By following thin layer chromatography, the fractions containing the same compound was spooled and dried. The compound was subjected to purification (purity >98%) by high-performance liquid chromatography (HPLC) using X-Terra RP column, No. 186000456 (2.1 × 150 mm, 5 μm) and isocratic elution was performed with methanol and distilled water (HPLC grade) (1:1) with 0.1% formic acid (flow rate 0.2 mL/min; injection volume 5 μL; retention time 7-8 minutes) and then crystallization was done. The crystals (melting point 175°C to 178°C) were characterized by nuclear magnetic resonance (Bruker Ascend 400MHz NMR), and mass spectroscopy using HPLC–mass spectrometry with water micromass ZQ detector. The resulting compound was characterized and identified as deoxyrhapontigenin (DR).
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3

NMR Spectroscopy Protocol for Solvent Referencing

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NMR data
were recorded with a Bruker Ascend 400 MHz NMR. The chemical shift
for 1H NMR spectra was reported in parts per million (ppm)
referenced to the characteristic solvent signal of CDCl3 at 7.26 ppm or DMSO-d6 at 2.49 ppm.
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