Column chromatography was carried out using silica gel (3.0 × 30 cm, Qingdao Marine, China), CHP20P (3.0 × 25 cm, Mitsubishi, Japan), octadecylsilyl silica (ODS) (YMC, Japan) and Sephadex LH-20 (1.5 × 180 cm, GE Healthcare, Sweden). Semi-preparative high performance liquid chromatography (HPLC) was conducted on a 1260 system (Agilent, USA) equipped with an XDB-C18 column (9.4 × 250 mm, 5 μm, Agilent, USA). Ultra violet (UV) spectra were determined using a 241 spectrophotometer (Perkin Elmer, USA). High resolution electrosparay ionization mass spectrum (HR-ESIMS) spectra were recorded on a 6545 Q-TOF instrument (Agilent, USA). Nuclear magnetic resonance (NMR) spectra were acquired using an AV-600 instrument (Bruker, Germany). Electronic circular dichroism (ECD) spectra were obtained using a MOS-450 instrument (Bio-Logic, France). The solvents used in column chromatography were analytical grade (Tianjin Hengxing, China), the solvents used in HPLC, HR-ESIMS, ECD and activity assays were chromatographic grade (Sigma-Aldrich, USA), and the solvent used in NMR was methanol-d4 (Cambridge Isotope Laboratories, USA).
Av 600 instrument
Manufactured by Bruker
Sourced in Germany
The AV-600 is a high-performance nuclear magnetic resonance (NMR) spectrometer produced by Bruker. It is designed to provide researchers with a powerful tool for the analysis and characterization of chemical compounds. The AV-600 operates at a frequency of 600 MHz and is capable of generating high-resolution NMR spectra.
Automatically generated - may contain errors
Lab products found in correlation
Sephadex lh 20, by GE Healthcare (2 mentions)
1260 system, by Agilent Technologies (2 mentions)
241 spectrophotometer, by PerkinElmer (2 mentions)
Mos 450 instrument, by Bio-Logic (1 mentions)
Xdb c18 column, by Agilent Technologies (1 mentions)
Methanol d4, by Cambridge Isotopes (1 mentions)
6545 q tof instrument, by Agilent Technologies (1 mentions)
Chp20p, by Mitsubishi (1 mentions)
Synergy 4 multi detection microplate reader, by Agilent Technologies (1 mentions)
A1 confocal laser microscope, by Nikon (1 mentions)
Ec c18 column, by Agilent Technologies (1 mentions)
Spectrum one perkin elmer spectrophotometer, by PerkinElmer (1 mentions)
Tensor 27 spectrometer, by Bruker (1 mentions)
Deuterated solvent, by Cambridge Isotopes (1 mentions)
Sephadex lh 20, by Cytiva (1 mentions)
Silica gel gf254, by Qingdao Marine Chemical (1 mentions)
Silica gel, by Qingdao Marine Chemical (1 mentions)
8 protocols using av 600 instrument
1
Separating Natural Compounds via Chromatography
2
Synthesis and Characterization of Ru Complexes Interacting with Amyloid-β Peptides
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All common chemicals were purchased from Aldrich and used without further purification. All Ru complexes, Ru-N-1 , Ru-N-2 , Ru-N-3 , and Ru-N-4 were synthesized as reported (Webb et al., 2012 (link)). The Aβ1−16, and Aβ1−42 peptides were purchased from 21st Century Biochemicals (Marlborough, MA, USA), and Cellmano Biotech Limited (Hefei, China), and monomerized before use according to a reported procedure (Sabate et al., 2003 (link); Pachahara et al., 2012 (link)). Aβ1−16 was dissolved in double distilled H2O (ddH2O), while Aβ1−42 was dissolved in DMSO and ddH2O in a 1:1 mixture, unless stated otherwise. The stock peptide solution concentration was determined by absorbance with the use of a Thermo Nicolet UV nanodrop and an extinction coefficient of 1,410 and 1,450 M−1cm−1 at 280 nm for Aβ1−16, and Aβ1−42 respectively (Guilloreau et al., 2007 (link); Coalier et al., 2013 (link)). Turbidity assays were measured using a Synergy 4 Multi-Detection microplate reader from BioTek. 1H NMR spectra were recorded on a Bruker AV-600 instrument. TEM images were obtained using an OSIRIS FEI scanning TEM (STEM) operating at 200 kV.
3
Purification of Target Compound from CBM Propolis
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The ethanol extract (ca. 30 g) of CBM propolis was fractionated by silica gel CC successively eluted with a gradient of increasing chloroform in methanol (10:1→0:1, v/v) and produced fractions A–E, the fraction B with a higher purity (>70%) of the target compound was subjected to Sephadex LH-20 (CHCl3/MeOH, 1:1, v/v, GE Healthcare Bio-Sciences AB, Uppsala, Sweden) and then separated further by preparative HPLC (Agilent 1260, Daisogel C-18 column (250 × 20 mm, 10 μm), MeOH/H2O = 27:73, v/v; 12 mL/min, 25 °C) to afford high purity of target product. The HPLC-ESI /MS procedures were implemented as above and the 1H NMR spectra were carried out on a Bruker AV-600 instrument (Bruker, Karlsruhe, Germany) with deuterated solvent signals used as internal standards to establish the structures of unknow compounds by comparison with reference data.
4
Isolation and Characterization of Natural Compounds
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Column chromatography was carried out using silica gel (Qingdao Marine, China), MCI (Mitsubishi, Japan), and Sephadex LH-20 (GE Healthcare, Sweden). RP-HPLC isolation was performed using a 1,260 system (Agilent, United States) coupled with a 250 mm × 10 mm, 5 μm XDB-C18 column (YMC, Japan). UV spectra were determined using a 241 spectrophotometer (Perkin Elmer, United States). HR-ESIMS spectra were measured using a 6,545 Q-TOF spectrometer (Agilent, United States). NMR spectra were recorded using an AV-600 instrument (Bruker, Germany). GC analysis was performed using a 7890A system (Agilent, United States). ECD spectra were obtained using a MOS-450 detector (Bio-Logic, France). Cell viability analyses were performed using an A1 laser confocal microscope (Nikon, Japan). UPLC-MS/MS analyses were performed using a 6,545 LC/Q-TOF system (Agilent, United States) coupled with a 50 mm × 2.1 mm, 1.9 μm EC-C18 column (Agilent, United States).
5
Isolation and Characterization of DMDD from Averrhoa carambola
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DMDD was prepared as previously described by Wen et al. [16 (link)], with a minor change. A powder from air-dried roots of Averrhoa carambola L. (12 kg) was extracted with 60% aq. EtOH under reflux three times (3 × 96 l, 1 h for each). The ethanol solution was concentrated under vacuum conditions to yield a syrup-like extract, which was suspended in H2O and then extracted with cyclohexane (3 × 20 l), EtOAc (3 × 20 l) and n-BuOH (3 × 20 l).
The cyclohexane extract (10.3 g) was subjected to open silica gel CC (3 × 80 cm, 200–300 mesh) via successive elution with a gradient of cyclohexane/EtOAc (100 : 0–0 : 100, each 200 ml) to yield seven fractions (fractions 1–7). Fraction 4 (5.0 g) was further separated by open silica gel CC (3 × 80 cm, 200–300 mesh) via successive elution with a gradient of cyclohexane/EtOAc (100 : 0–15 : 1, each 100 ml), producing 4 sub-fractions (fractions 41–44). Fraction 44 was re-crystallized with MeOH to yield 2-dodecyl-6-methoxycyclohexa-2,5-diene-1,4-dione (2350 mg). This compound was identified by FTIR spectroscopy using a Spectrum One PerkinElmer spectrophotometer and by 1H and 13C NMR analysis on a Bruker AV 600 instrument. The chemical structure of DMDD is illustrated below (Figure 1 ).
The cyclohexane extract (10.3 g) was subjected to open silica gel CC (3 × 80 cm, 200–300 mesh) via successive elution with a gradient of cyclohexane/EtOAc (100 : 0–0 : 100, each 200 ml) to yield seven fractions (fractions 1–7). Fraction 4 (5.0 g) was further separated by open silica gel CC (3 × 80 cm, 200–300 mesh) via successive elution with a gradient of cyclohexane/EtOAc (100 : 0–15 : 1, each 100 ml), producing 4 sub-fractions (fractions 41–44). Fraction 44 was re-crystallized with MeOH to yield 2-dodecyl-6-methoxycyclohexa-2,5-diene-1,4-dione (2350 mg). This compound was identified by FTIR spectroscopy using a Spectrum One PerkinElmer spectrophotometer and by 1H and 13C NMR analysis on a Bruker AV 600 instrument. The chemical structure of DMDD is illustrated below (
6
Synthesis and Characterization of Novel Compounds
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All reactions were performed in open atmosphere unless stated. All reagents, unless otherwise indicated, were obtained from commercial sources. 1H and 13C NMR spectra were recorded on a Bruker AV-600 instrument or Variance 400 spectrometer with DMSO-d6 or CDCl3 as solvent and tetramethylsailane (TMS) was used as internal standard (δ in ppm). IR spectra were obtained on a Bruker Tensor 27 spectrometer (KBr disc). HRMS were recorded on a Bruker UHR-TOF maXis spectrometer. X-ray data were collected on a Bruker Smart APEX-2 diffractometer. Melting points were taken on a hot-plate microscope apparatus and were uncorrected.
7
Characterization of Organic Compounds
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All reagents and solvents were purchased from Energy Chemical Co (Shanghai, China). Nuclear magnetic resonance (NMR) spectra were obtained using a Bruker AV-600 instrument (Bruker, Karlsruhe, Germany). Deuterated solvents were obtained from Cambridge Isotope Laboratories (Andover, MA, USA). DMSO-d6 and CDCl3 solvent peaks (2.50 and 7.26 ppm for 1H and 39.52 and 77.16 ppm for 13C, respectively) were used as internal chemical shift references. Mass spectrographic analysis was conducted on a Waters SYNAPTQTM (Waters, Milford, MA, USA). Analytical thin-layer chromatography (TLC) was carried out on percolated plates (silica gel GF254), and spots were visualized with ZF-20D ultraviolet analyzer (Qingdao Marine Chemical Ltd., Qingdao, China). Silica gel (200–300 mesh) was used for column chromatography.
8
Chromatographic Techniques for Natural Product Isolation
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Silica gel (100–200 and 200–300 mesh) for column chromatography (CC) and GF254 Silica gel for thin layer chromatography (TLC) were purchased from Qingdao Marine Chemical Ltd., Qingdao, China. Sephadex LH-20 obtained from Amersham Biosciences, Sweden was used for CC. Other reagents were of analytical grade purchased from Guangzhou reagent Co. Ltd. NMR spectra (1H, 13C-NMR) were determined on a Bruker AV-600 instrument using TMS as an internal reference.
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