All common solvent and reagents were obtained by commercial sources. NMR spectra were recorded on Bruker Avance III 700 MHz and these were used both for quality control and to verify the concentration of the stock solutions used for dose response measurements and in vivo studies. An Agilent LC-TOF instrument was used to obtain high-resolution mass spectral data. Purification of all agents was obtained using RP-HPLC on a JASCO preparative system equipped with a PDA detector. The instrument is also equipped with a fraction collector controlled by a ChromNAV system (JASCO). For all agents, a Luna C18 10μ 10 × 250mm (Phenomenex) column was used to purify agents to > 95% purity. For intermediate reagents that were not commercially available, RP-chromatography purification was performed using a CombiFlash (Teledyne ISCO). GM6001 was obtained from Enzo Life science. MMP408 was obtained from EMD Millipore Corp.
Chromnav system
Manufactured by Jasco
The ChromNAV system is a chromatography data system that enables the acquisition, analysis, and management of chromatographic data. It provides a comprehensive software solution for various analytical techniques, including high-performance liquid chromatography (HPLC), gas chromatography (GC), and other related methods.
Automatically generated - may contain errors
Lab products found in correlation
Avance 3 700 mhz, by Bruker (3 mentions)
Luna c18 10μ 10 250mm, by Phenomenex (2 mentions)
Mmp408, by Merck Group (1 mentions)
Gm6001, by Enzo Life Sciences (1 mentions)
Combiflash, by Teledyne (1 mentions)
Luna c18, by Phenomenex (1 mentions)
Combiflash rf, by Teledyne (1 mentions)
Lcl161, by MedChemExpress (1 mentions)
Sephacryl s 200, by Cytiva (1 mentions)
Md 4010, by Jasco (1 mentions)
6 protocols using chromnav system
1
Analytical Characterization of Small Molecules
2
Peptide Purification and Characterization
3
Analytical Characterization of Novel Compounds
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All reagents and solvents were obtained
from commercial sources, including the majority of Fmoc-protected
amino acids and resins for solid-phase synthesis. NMR spectra in DMSO-d6 were used to evaluate the concentration of
stock solutions and were recorded on a Bruker Avance III 700 MHz equipped
with a TCI cryoprobe. 1H NMR measurements in assay buffer
were used for quality control and to routinely verify the solubility
of the compounds used for all studies. High-resolution mass spectral
data were acquired on an Agilent 6545 Q-TOF LC/MS instrument (Table S4 ). RP-HPLC purifications were performed
on a JASCO preparative system equipped with a PDA detector and a fraction
collector controlled by a ChromNAV system (JASCO) on an XTerra C18
10 μm 10 × 250 mm2 (Waters). The purity of tested
compounds was assessed by HPLC. All compounds had a purity of ≥95%
(Figures S10–S12 ).
from commercial sources, including the majority of Fmoc-protected
amino acids and resins for solid-phase synthesis. NMR spectra in DMSO-d6 were used to evaluate the concentration of
stock solutions and were recorded on a Bruker Avance III 700 MHz equipped
with a TCI cryoprobe. 1H NMR measurements in assay buffer
were used for quality control and to routinely verify the solubility
of the compounds used for all studies. High-resolution mass spectral
data were acquired on an Agilent 6545 Q-TOF LC/MS instrument (
on a JASCO preparative system equipped with a PDA detector and a fraction
collector controlled by a ChromNAV system (JASCO) on an XTerra C18
10 μm 10 × 250 mm2 (Waters). The purity of tested
compounds was assessed by HPLC. All compounds had a purity of ≥95%
(
4
Preparative RP-HPLC Purification of Compounds
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RP-HPLC purification was performed
on a JASCO preparative system equipped with a PDA detector and a fraction
collector controlled by a ChromNAV system (JASCO) on an XTerra C18
10 μm 10 × 250 mm2 (Waters). The purity of tested
compounds was assessed by HPLC (purity > 95%).155H1 purity
analysis is reported inFigure S27 (purity
of >98%).
on a JASCO preparative system equipped with a PDA detector and a fraction
collector controlled by a ChromNAV system (JASCO) on an XTerra C18
10 μm 10 × 250 mm2 (Waters). The purity of tested
compounds was assessed by HPLC (purity > 95%).
analysis is reported in
of >98%).
5
Analytical Methods for LCL161 Characterization
6
Chiral Separation of Single-Walled Carbon Nanotubes
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Chiral index dependent separation was performed using gel chromatography. Approximately 2.0 mg of SWNTs were added to a vial containing 2.5 mL of aqueous 1.0 wt% SC (≥98%). The vial was bath-sonicated for 3 h (Branson; Bransonic Ultrasonic Cleaner 2510J-MT). The resulting dispersion was centrifuged at 140,000 × g for 1 h in a high-speed centrifuge equipped with an S58A angle rotor (Koki Holdings Co., Ltd.; micro ultracentrifuge CS 100FNX). 2.0 mL of aqueous 2.0 wt% SDS (≥97%) was added to the supernatant solution before the HPLC separation. The helicity sorting and optical resolution of the SWNTs were achieved via HPLC using a JASCO ChromNAV system equipped with a JASCO LC-Net II interface, a JASCO PU-2089i gradient inert pump, a JASCO MD-4010 photo diode array detector, a CO-4060 column oven (23 °C), and a column (ϕ10 × 200 mm) filled with the gel (Sephacryl S-200, Cytiva). The flow rate was 2.0 mL min−1 and the sample (SWNTs dispersion) injection volume was 3 mL. The eluent was an aqueous solution containing 0.5 wt% SC + 0.5 wt% SDS + X wt% DOC (>96%). The concentration of DOC (X) increased from 0 to 1. Fractions were collected every 5 mL using a fraction collector.
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