1H- and 13C-NMR, COSY, HSQC, HMBC, and NOESY data were obtained using a superconducting FT-NMR 400 or 500 MHz spectrometer (Agilent Technologies, Santa Clara, CA, USA). HR-ESI mass spectra were recorded on an Agilent Technologies, 6530 Accurate-Mass Q-TOF LC/MS. The HPLC system (Shimadzu, Tokyo, Japan) consisted of a UV/VIS detector (model SPD-20A), two pumps (model LC-20AT), a system controller (model CBM-20A) and a workstation (model HW-2000 solution). Column chromatography was performed using Sephadex LH-20 gel (25–100 μM mesh, Pharmacia, Stockholm, Sweden) and silica gel (230–400 mesh, Merck, Darmstadt, Germany).
6530 accurate mass q tof lc ms
Manufactured by Agilent Technologies
Sourced in United States
The 6530 Accurate-Mass Q-TOF LC/MS is a high-resolution, high-mass accuracy liquid chromatography-mass spectrometry (LC/MS) system. It is designed to provide precise mass measurements and sensitive detection of compounds in complex samples.
Automatically generated - may contain errors
Lab products found in correlation
Silica gel, by Merck Group (4 mentions)
Avance 3 nmr spectrometer, by Bruker (3 mentions)
Hplc system, by Shimadzu (2 mentions)
Cbm 20a, by Shimadzu (2 mentions)
Hplc system, by Phenomenex (2 mentions)
Luna c18, by Phenomenex (2 mentions)
600 mhz spectrometer, by Bruker (2 mentions)
P 2000 polarimeter, by Jasco (2 mentions)
Multiskan go, by Thermo Fisher Scientific (2 mentions)
Spd 20a, by Shimadzu (1 mentions)
Lc 20at, by Shimadzu (1 mentions)
1260 lc system, by Agilent Technologies (1 mentions)
Extend c18 rp uplc column, by Agilent Technologies (1 mentions)
Chemstation, by Agilent Technologies (1 mentions)
Avance 3, by Bruker (1 mentions)
Mercury plus, by Agilent Technologies (1 mentions)
Vertex 70v ftir spectrophotometer, by Bruker (1 mentions)
Kieselgel 60 f254 aluminum sheets, by Merck Group (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Melting point apparatus, by Büchi (1 mentions)
43 protocols using 6530 accurate mass q tof lc ms
1
Spectroscopic Characterization of Compounds
2
Extracting and Analyzing Crude Extracts
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The supernatant and pellets were extracted with ethyl acetate (1:1, v/v). The extracts were dried with Na2SO4 and evaporated to dryness under reduced pressure to yield crude extracts. After being weighed, the extracts were dissolved in methanol to obtain a final concentration of 1 mg/mL. LC and LC-MS/MS analyses were carried out after filtration through 0.2-μm Acrodisc MS syringe filters (25 mm).
The samples were injected as 20 μL into an Agilent 1260 LC system with an Agilent Extend-C18 RP UPLC column (2.1 × 100 mm, 1.8 μm) connected to an Agilent 6530 Accurate-Mass Q-TOF LC/MS. The LC gradient was as follows: 10% (v/v) acetonitrile (ACN) (0.1% water, 0–3 min), 10–100% (v/v) ACN (0.1% water)/0.1% water (3–23 min), 100% ACN (0.1% water, 23–25 min), 10% (v/v ACN (0.1% water, 25–30 min). The column compartment temperature was 25 °C.
Q-TOF MS settings during the LC gradient were as follows: acquisition mass range m/z 100–1600, MS scan rate 1s-1, MS/MS scan rate 2s-1, fixed collision energy 20 eV, source-gas temperature 300 °C, gas flow 11 L min-1, nebulizer 45 psi, ion polarity positive; scan source parameters—VCap 3000, Fragmentor 100, Skimmer1 65, OctopoleRFPeak 750. The MS was autotuned using Agilent tuning solution in positive mode before each measurement. LC (DAD) and MS data were analyzed with ChemStation and MassHunter software (Agilent), respectively.
The samples were injected as 20 μL into an Agilent 1260 LC system with an Agilent Extend-C18 RP UPLC column (2.1 × 100 mm, 1.8 μm) connected to an Agilent 6530 Accurate-Mass Q-TOF LC/MS. The LC gradient was as follows: 10% (v/v) acetonitrile (ACN) (0.1% water, 0–3 min), 10–100% (v/v) ACN (0.1% water)/0.1% water (3–23 min), 100% ACN (0.1% water, 23–25 min), 10% (v/v ACN (0.1% water, 25–30 min). The column compartment temperature was 25 °C.
Q-TOF MS settings during the LC gradient were as follows: acquisition mass range m/z 100–1600, MS scan rate 1s-1, MS/MS scan rate 2s-1, fixed collision energy 20 eV, source-gas temperature 300 °C, gas flow 11 L min-1, nebulizer 45 psi, ion polarity positive; scan source parameters—VCap 3000, Fragmentor 100, Skimmer1 65, OctopoleRFPeak 750. The MS was autotuned using Agilent tuning solution in positive mode before each measurement. LC (DAD) and MS data were analyzed with ChemStation and MassHunter software (Agilent), respectively.
3
Spectroscopic Analysis of Organic Compounds
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All reagents and anhydrous solvents were purchased from Sigma-Aldrich, Alpha, Acros, and Merck and used without further purification. The 1H NMR and 13C NMR spectra were recorded on a Bruker (Avance III) 400 MHz NMRspectrometer. The FT-IR spectrum was recorded with a Perkin Elmer spectrophotometer using an ATR head in the range of 4000–600 cm−1. Melting point (M.p.) was measured with a Thermo Scientific melting point device. The mass spectra were recorded on an Agilent Technologies 6530 Accurate-Mass Q-TOF LC/MS.
4
Spectroscopic Characterization of Compounds
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NMR spectra were recorded on a Varian Mercury Plus at 400 MHz for 1 H NMR and 100 MHz for 13 C NMR by using TMS as the internal standard. The solvents were CDCl3. HR-ESI-MS was performed on Agilent 6530 Accurate- Mass Q-TOF LC/MS. UV spectra were measured using Thermo Scientific Multiskan GO microplate and cuvette spectrophotometer. IR spectra were run on a Bruker VERTEX 70v FT-IR Spectrophotometer. Column chromatographies were performed on Silica gel 60 (0.063–0.200 mm, Merck) and Sephadex LH-20 (Fluka). TLC was carried out on pre-coated Kieselgel 60 F254 aluminum sheets (Merck).
5
Synthesis of Iron-Catalyzed Organic Compounds
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All reactions were carried out in oven-dried glassware using dry solvents under a molecular oxygen atmosphere, unless stated otherwise. Iron salts were purchased from Sigma-Aldrich and were used as received. All other chemicals were used as received from commercial sources. Reactions were monitored via TLC on 0.25 mm Merck silica gel plates (60 F254) using UV light for visualization. Column chromatography purification was performed using silica gel (100–200 mesh). Melting points were measured using Büchi melting point apparatus and are uncorrected. IR spectra were recorded using a Spectrum FT-IR spectrophotometer. NMR spectra were recorded using a Bruker 400 MHz spectrometer (1H: 400 MHz, 13C: 100 MHz), using DMSO-d6 or CDCl3 as the solvent with TMS as the internal standard at room temperature. Mass spectra were recorded using a 6530 Accurate-Mass Q-TOF LC/MS (Agilent Technologies).
6
Peptide Synthesis and Characterization
7
Synthesis and Photodynamic Activity of BOD Dyes
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All reagents and solvents were purchased
from commercial sources and used without further purification. CompoundsBOD1 and BOD2 were prepared using the literature
procedures.24 (link),27 (link) Column chromatography was carried
out using a silica stationary phase (230–400 mesh, SiliCycle
Inc., Canada). Analytical thin layer chromatography was performed
on 0.25 mm thick precoated silica gel plates (60F254, Merck, Germany).
Compounds were visualized under UV light. All 1H NMR spectra
were recorded on a Varian Inova instrument (400 MHz) at Selçuk
University, Konya. Chemical shifts (δ) are reported in parts
per million (ppm) and referenced to the residual solvent peak. Coupling
constants (J) are reported in hertz (Hz). Standard
abbreviations indicating multiplicities are given: br = broad, d =
doublet, m = multiplet, s = singlet, and t = triplet. High-resolution
mass spectrometry was carried out using an Agilent 6530 Accurate-Mass
Q-TOF LC/MS of the Eastern Anatolia Advanced Technology Research and
Application Centre (DAYTAM, Erzurum, Turkey). For PDT, an LED from
Bright LED Electronics Corp., model BL-BG43V4V, with peak absorption
value at 506 nm was used as a light source. For cell culture experiments
DLD-1 human colorectal adenocarcinoma cells (ATCC) were used.
from commercial sources and used without further purification. Compounds
procedures.24 (link),27 (link) Column chromatography was carried
out using a silica stationary phase (230–400 mesh, SiliCycle
Inc., Canada). Analytical thin layer chromatography was performed
on 0.25 mm thick precoated silica gel plates (60F254, Merck, Germany).
Compounds were visualized under UV light. All 1H NMR spectra
were recorded on a Varian Inova instrument (400 MHz) at Selçuk
University, Konya. Chemical shifts (δ) are reported in parts
per million (ppm) and referenced to the residual solvent peak. Coupling
constants (J) are reported in hertz (Hz). Standard
abbreviations indicating multiplicities are given: br = broad, d =
doublet, m = multiplet, s = singlet, and t = triplet. High-resolution
mass spectrometry was carried out using an Agilent 6530 Accurate-Mass
Q-TOF LC/MS of the Eastern Anatolia Advanced Technology Research and
Application Centre (DAYTAM, Erzurum, Turkey). For PDT, an LED from
Bright LED Electronics Corp., model BL-BG43V4V, with peak absorption
value at 506 nm was used as a light source. For cell culture experiments
DLD-1 human colorectal adenocarcinoma cells (ATCC) were used.
8
Spectroscopic Characterization of Organic Compounds
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ESI-HRMS (positive) spectra were documented on Agilent Technologies (6530, Accurate Mass Q-TOF LC/MS). ATR-FTIR (solid) spectra were recorded on a Bruker, ATR-Tensor 37 spectrophotometer with wave numbers (ν) in cm−1. Optical rotations were recorded on a KRUSS P3000 polarimeter purchased from A. Kruss Optronic, Germany. The 1H (600 MHz) and 13C (150 MHz) NMR spectra were measured on BRUKER AVANCE NMR spectrometers (600 MHz) using solvent peaks (CDCl3, δH: 7.26; δC: 77.0), (CD3OD, δH: 4.87; δC: 48.5) as internal reference. Data were reported in the following order: multiplicities are indicated as s = singlet, m = multiplet, t = triplet, dd = doublet of doublet, d = doublet; chemical shift (δ) in ppm; coupling constants (J) are in hertz (Hz). Column chromatography was applied by using 100–200 mesh silica gel. For thin layer chromatography, pre-coated aluminum sheets (silica gel 60F-254, E. Merck) were used. The compounds were visualization with UV-light (254 and 366 nm) or I2 stain and also by spraying with the ceric sulfate reagent.
9
Untargeted Metabolomics Using Q-TOF LC/MS
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The untargeted metabolomics analysis of samples was performed using an Agilent Technologies 6530 Accurate-Mass Q-TOF LC/MS (USA).
10
Standardized Protein Characterization Methods
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