The isolation of compounds from A. nomius NC06 involved several instruments including chromatographic methods consisting of both analytical and semipreparative HPLC, NMR spectroscopy, and ESIMS. HPLC analysis was carried out on a Dionex Ultimate 3000 system with a C18 column, 4.6 × 150 mm, 5 µm, mobile phase A: H2O with 0.1% TFA; B: methanol, flow rate: 1 mL/min. Gradient elution from 0 to 35 min was 10–100% B, then washed at 100% B from 35 to 45 min and equilibrated back to 10% B from 46 to 60 min. Semipreparative HPLC was carried out with a Merck Hitachi Chromaster HPLC system. The chromatography method was conducted with silica gel 60 M for VLC and Sephadex LH-20 for column chromatography. The purity of the isolated compound was monitored by TLC using silica gel 60 F254 by using DCM and 5% MeOH as mobile phase. The 1D and 2D NMR spectra were recorded on a Bruker AVANCE DMX 600 NMR spectrometer. The chemical shifts (δ) were referenced to the residual solvent signals (DMSO-d6: δH 2.50/δC 39.5). ESIMS spectra were acquired on a Finnigan LCQ Deca mass spectrometer. HRESIMS spectra were measured with a UHR-QTOF maXis 4G (Bruker Daltonics) mass spectrometer.
Uhr qtof maxis 4g
Manufactured by Bruker
The UHR-QTOF maXis 4G is a high-performance quadrupole time-of-flight (Q-TOF) mass spectrometer designed for ultra-high-resolution accurate mass analysis. It features a high-capacity dual linear ion trap, an advanced quadrupole mass filter, and a high-resolution orthogonal acceleration time-of-flight analyzer.
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Lab products found in correlation
Ultimate 3000 system, by Thermo Fisher Scientific (2 mentions)
Avance dmx 600, by Bruker (2 mentions)
P 2000 polarimeter, by Jasco (2 mentions)
Avance dmx600 nmr spectrometer, by Bruker (1 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)
Eurospher 100 10 c18, by Knauer (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)
3 protocols using uhr qtof maxis 4g
1
Isolation and Characterization of A. nomius Compounds
2
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.
3
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.
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