Electrochemical tests were carried out with a potentiostat (Metrohm μAutolab II). Three-electrode measurements have been employed in which glassy carbon disk electrode (Ø 3 mm), Pt wire, and KCl-saturated calomel electrode (SCE, Radiometer REF 401) acted as the working electrode, counter electrode, and reference electrode, respectively. Phosphoric acid solution and solid sodium hydroxide were introduced to make phosphate buffer solutions with different pH values monitored with a pH meter (Jenway 3505). Qualitative and quantitative analysis of the catechin and quercetin release experiments was accomplished with liquid chromatography-mass spectroscopy (LC-MS) technique employing an Agilent 6545 Accurate-Mass Q-TOF LC/MS system. Scanning electron microscopy (SEM) images were captured with JEOL JSM-6301F FESEM equipment.
6545 accurate mass q tof lc ms system
Manufactured by Agilent Technologies
The 6545 Accurate-Mass Q-TOF LC/MS system is a high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF MS) instrument. It is designed to provide accurate mass measurements and high-resolution separation of complex samples. The system combines a quadrupole mass analyzer and a time-of-flight mass analyzer to deliver precise mass data for qualitative and quantitative analysis.
Automatically generated - may contain errors
Lab products found in correlation
Prep lc system, by Waters Corporation (2 mentions)
μautolab 2, by Metrohm (1 mentions)
Autopol 4 polarimeter, by Rudolph Research Analytical (1 mentions)
Milli q pf filtered, by Merck Group (1 mentions)
Gx 281, by Waters Corporation (1 mentions)
Cary 50 bio uv vis spectrophotometer, by Agilent Technologies (1 mentions)
Milli q pf, by Merck Group (1 mentions)
5 mm cpp tci cryo probe, by Bruker (1 mentions)
Hplc purificationsystem, by Gilson (1 mentions)
Avance 3 hd spectrometer, by Bruker (1 mentions)
600 mhz spectrometer, by Bruker (1 mentions)
4 protocols using 6545 accurate mass q tof lc ms system
1
Electrochemical and Analytical Characterization
2
Analytical Techniques for Chemical Characterization
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General Experimental
Procedures. Optical rotations were recorded on a Rudolph Research
Analytical Autopol IV polarimeter using a 0.25 dm cell in the solvent
indicated. NMR spectra were recorded at 25 °C on a 400 MHz Agilent
Inova spectrometer equipped with a 5 mm OneNMR probe. The 1H and 13C NMR chemical shifts were referenced to the solvent
peaks for CDCl3 at δH 7.26 and δC 77.0. NMR FID processing and data interpretation was done
using MestReNova software, version 14.0. High-resolution mass spectra
were recorded on an Agilent 6545 Accurate-Mass Q-TOF LC/MS system
(1290 Infinity II) equipped with a dual AJS ESI source. Preparative-scale
HPLC purification was performed with a Waters Prep LC system, equipped
with a Delta 600 pump and a 996-photodiode array detector using the
Phenomenex Kinetex C8 HPLC column [5 μm, 150 ×
21.2 mm]. All solvents used for chromatography, UV, and MS were HPLC
grade, and the H2O was Millipore Milli-Q PF filtered.
Procedures. Optical rotations were recorded on a Rudolph Research
Analytical Autopol IV polarimeter using a 0.25 dm cell in the solvent
indicated. NMR spectra were recorded at 25 °C on a 400 MHz Agilent
Inova spectrometer equipped with a 5 mm OneNMR probe. The 1H and 13C NMR chemical shifts were referenced to the solvent
peaks for CDCl3 at δH 7.26 and δC 77.0. NMR FID processing and data interpretation was done
using MestReNova software, version 14.0. High-resolution mass spectra
were recorded on an Agilent 6545 Accurate-Mass Q-TOF LC/MS system
(1290 Infinity II) equipped with a dual AJS ESI source. Preparative-scale
HPLC purification was performed with a Waters Prep LC system, equipped
with a Delta 600 pump and a 996-photodiode array detector using the
Phenomenex Kinetex C8 HPLC column [5 μm, 150 ×
21.2 mm]. All solvents used for chromatography, UV, and MS were HPLC
grade, and the H2O was Millipore Milli-Q PF filtered.
3
Comprehensive Spectroscopic Characterization of Compounds
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IR spectra
were recorded as a dry film on a Bruker Alpha II spectrometer or a
Bruker Invenio S spectrometer equipped with an HTS-XT accessory. UV
spectra were recorded as methanol solutions on a Varian Cary 50-Bio
UV/vis spectrophotometer. NMR spectra were recorded at 25 °C
on a 600 MHz Bruker Avance III HD spectrometer, equipped with a triple
resonance 5 mm CPP TCI cryo-probe, and operating at a frequency of
600.0 MHz for the 1H nucleus and 150.9 MHz for the 13C nucleus. All 2D NMR experiments were acquired with non-uniform
sampling (NUS) set to 40% (for 1H–1H
detected experiments) or 35% (for 1H–13C detected experiments). 1H and 13C NMR chemical
shifts were referenced to the solvent peak for DMSO-d6 at δH 2.50 δC 39.50.
NMR FID processing and data interpretation was done using MestReNova
software, version 14.2. High-resolution mass spectra were recorded
on an Agilent 6545 Accurate-Mass Q-TOF LC/MS system (1290 Infinity
II) equipped with a dual AJS ESI source. Semi-preparative scale HPLC
purification was performed with either a Gilson HPLC purification
system equipped with a GX-281 liquid handler, a 322-binary pump, and
a 172-photodiode array detector or a Waters Prep LC system, equipped
with a Delta 600 pump and a 996-photodiode array detector. All solvents
used for chromatography, UV, and MS were HPLC grade, and the H2O was Millipore Milli-Q PF filtered.
were recorded as a dry film on a Bruker Alpha II spectrometer or a
Bruker Invenio S spectrometer equipped with an HTS-XT accessory. UV
spectra were recorded as methanol solutions on a Varian Cary 50-Bio
UV/vis spectrophotometer. NMR spectra were recorded at 25 °C
on a 600 MHz Bruker Avance III HD spectrometer, equipped with a triple
resonance 5 mm CPP TCI cryo-probe, and operating at a frequency of
600.0 MHz for the 1H nucleus and 150.9 MHz for the 13C nucleus. All 2D NMR experiments were acquired with non-uniform
sampling (NUS) set to 40% (for 1H–1H
detected experiments) or 35% (for 1H–13C detected experiments). 1H and 13C NMR chemical
shifts were referenced to the solvent peak for DMSO-d6 at δH 2.50 δC 39.50.
NMR FID processing and data interpretation was done using MestReNova
software, version 14.2. High-resolution mass spectra were recorded
on an Agilent 6545 Accurate-Mass Q-TOF LC/MS system (1290 Infinity
II) equipped with a dual AJS ESI source. Semi-preparative scale HPLC
purification was performed with either a Gilson HPLC purification
system equipped with a GX-281 liquid handler, a 322-binary pump, and
a 172-photodiode array detector or a Waters Prep LC system, equipped
with a Delta 600 pump and a 996-photodiode array detector. All solvents
used for chromatography, UV, and MS were HPLC grade, and the H2O was Millipore Milli-Q PF filtered.
4
Purification and Characterization of Organic Compounds
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The reagents and solvents were purchased from commercial companies, such as Adamas-beta®, Bide pharmatech etc., and used without further purification. The nonaqueous reactions were performed under nitrogen atmosphere. The reactions were monitored by Shimadzu 8040 quadrupole LC/MS system or TLC and terminated as judged by the consumption of the starting material. Flash chromatography was performed on silica gel (200–300 mesh) using SepaBean® machine and visualized under UV light monitor. 1HNMR (600 MHz) and 13CNMR (150 MHz) spectra were measured on Bruker 600 MHz spectrometer using TMS as internal standard at ambient temperature. The chemical shifts (δ) were described as parts per million (ppm) downfield and coupling constants (J) values were expressed as hertz (Hz). High-resolution mass spectra (HRMS) data were reported by Agilent 6545 Accurate-Mass QTOF LC/MS system.
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