The NMR spectra were recorded with a Bruker Avance 500 MHz spectrometer. The high resolution mass spectra were recorded with a Bruker Daltonics microTOF-Q instrument. The LC-MS chromatograms were recorded with a Agilent Technologies 1260 Infinity Binary LC and Agilent 6100 Series Quadrupole LC/MS Systems with Phenomemex 150 × 4.6 SynergiTM 4 μm Fusion-RP 80 Å analytical column (flow rate 0.5 ml/min and wavelength 260 nm, 0.1% formic acid in H2O and MeCN as eluents).
Microtof q instrument
Manufactured by Bruker
Sourced in Germany, United States
The MicroTOF-Q instrument is a high-performance mass spectrometer designed for precise molecular analysis. It utilizes time-of-flight (TOF) technology coupled with a quadrupole mass filter to provide accurate mass measurements and efficient ion separation.
Automatically generated - may contain errors
Lab products found in correlation
Esi l low concentration tuning mix, by Agilent Technologies (5 mentions)
Avance 500, by Bruker (3 mentions)
Avance 300, by Bruker (2 mentions)
Ch2cl2, by Merck Group (2 mentions)
Series 1100 hplc pump, by Agilent Technologies (2 mentions)
Avance 500 mhz spectrometer, by Bruker (1 mentions)
1260 infinity binary lc, by Agilent Technologies (1 mentions)
Autoflex 3, by Bruker (1 mentions)
Microtof q11, by Bruker (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Silica gel, by GE Healthcare (1 mentions)
Uv 1700 spectrometer, by Shimadzu (1 mentions)
Av 500 spectrometer, by Bruker (1 mentions)
J w hp 5ms gc column, by Agilent Technologies (1 mentions)
Agilent 1100 series hplc instrument, by Agilent Technologies (1 mentions)
7890a gc system, by Agilent Technologies (1 mentions)
Squid vsm, by Quantum Design (1 mentions)
Zetasizer 90, by Malvern Panalytical (1 mentions)
Evolution 220 spectrophotometer, by Thermo Fisher Scientific (1 mentions)
Amx 500 nmr spectrometer, by Bruker (1 mentions)
26 protocols using microtof q instrument
1
NMR, HRMS, and LC-MS Analysis
2
Purification and Characterization of Organic Compounds
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Chemical reagents were obtained from commercial suppliers, and were dried and purified by standard methods when necessary. The progress of reactions was monitored by thin layer chromatography (TLC) using silica gel plates. The 1H-NMR and 13C-NMR spectra were recorded on a Bruker (Bruker, Rheinstetten, Germany) AVANCE III400 Hz spectrometer using CDCl3 or DMSO-d6 as solvent. Tetramethylsilane (δ = 0.00 ppm) was used as an internal standard. HRMS data were obtained using Bruker micrOTOF-Q instrument or TOF-MS instrument.
3
NMR and HRMS Characterization of Porphyrin Compounds
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NMR spectra were recorded
using a DRX 400 MHz Bruker NMR spectrometer
at 298 K. The chemical shifts are reported in parts per million (ppm)
relative to the residual proton signal (for 1H NMR) and
the carbon signal for (13C NMR) of the deuterated solvent
used [1H NMR: CDCl3 (7.26 ppm), DMSO-d6 (2.50 ppm); 13C NMR: CDCl3 (77.16 ppm), DMSO-d6 (39.52 ppm)]. The
acetone peak (2.22 ppm) was used as the internal reference for D2O as solvents, and all coupling constants are reported in
Hertz. The identification of aromatic protons characteristic for the
porphyrin and chlorin ring systems has previously been described.27 (link) A Bruker Autoflex III or a Bruker micro TOF-Q11
was used to obtain mass spectra. The molecular masses were determined
by high-resolution mass spectrometry (HRMS) recorded on a Bruker micrOTOF-Q
instrument with electrospray ionization.
using a DRX 400 MHz Bruker NMR spectrometer
at 298 K. The chemical shifts are reported in parts per million (ppm)
relative to the residual proton signal (for 1H NMR) and
the carbon signal for (13C NMR) of the deuterated solvent
used [1H NMR: CDCl3 (7.26 ppm), DMSO-d6 (2.50 ppm); 13C NMR: CDCl3 (77.16 ppm), DMSO-d6 (39.52 ppm)]. The
acetone peak (2.22 ppm) was used as the internal reference for D2O as solvents, and all coupling constants are reported in
Hertz. The identification of aromatic protons characteristic for the
porphyrin and chlorin ring systems has previously been described.27 (link) A Bruker Autoflex III or a Bruker micro TOF-Q11
was used to obtain mass spectra. The molecular masses were determined
by high-resolution mass spectrometry (HRMS) recorded on a Bruker micrOTOF-Q
instrument with electrospray ionization.
4
Comprehensive Analytical Techniques for Compound Characterization
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The UV spectra were measured on a Shimadzu UV-1700 spectrometer (Shimadzu Corporation, Kyoto, Japan). The IR spectra were measured on a Nicolet 10 Microscope Spectrometer (Thermo Scientific, San Jose, CA, USA). The 1D and 2D-NMR spectra were recorded on Bruker-AC (E)-500 spectrometer (Bruker AM 500, Fällanden, Switzerland) using tetramethylsilane (TMS) as an internal standard. The HR-ESI-MS was determined on a Bruker microTOF-Q instrument (Bruker BioSpin, Rheinstetten, Germany). Column chromatography was performed with silica gel (200–300 mesh; Qingdao Marine Chemical Inc., Qingdao, China), sephadex LH-20 (GE Healthcare), and ODS (50 µm; YMC Co. LTD., Kyoto, Japan). Preparative high performance liquid chromatography (HPLC) separations were performed on a SEP system (Beijing Sepuruisi scientific Co., Ltd., China) equipped with a variable-wavelength UV detector, using a YMC-Pack ODS-A column (250 × 20 mm, 5 μm). Chemical reagents for isolation were of analytical grade and purchased from Tianjin Siyou Co., Ltd., China. Biological reagents were from Sigma Company. Human heptocellular (HepG2), and breast (MCF-7) cancer cell lines were from Institute of Materia Medica, Chinese Academy of Medical Sciences and Peking Union Medical College, China.
5
Optimized Organic Synthesis Techniques
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Chemicals were purchased from Sigma-Aldrich
or Fluorochem and were used without purification. Solvents were purchased
from VWR Chemicals (CH2Cl2) or Sigma-Aldrich
[toluene, dioxane, and dimethyl sulfoxide (DMSO)] and used without
purification unless stated otherwise. Dry solvents were dried over
an inert PS-MD-5 solvent purification system, equipped with an activated
alumina/copper wire column. Microwave reactions were performed in
a closed vessel in a Biotage Initiator, measuring temperature by IR. 1H NMR measurements were acquired on a Bruker AVANCE 300 (300.13
MHz) or Bruker AVANCE 500 (500.23 MHz) spectrometer. 13C NMR measurements were acquired on a Bruker AVANCE 500 (125.78 MHz)
spectrometer. Chemical shifts are reported in parts per million downfield
of tetramethylsilane and are corrected according to the solvent. Mass
analysis was performed using a Bruker MicrOTOF-Q instrument on a positive
ion polarity mode for ESI (electrospray ionization). Capillary charge:
4000 V. Melting points were measured using a Büchi M-565 melting
point apparatus. SiO2 column chromatography was performed
using Merck silica gel C60 (particle size 40–60 μm).
Thin-layer chromatography (TLC) was performed on Merck silica gel
C60 F254 plates (silica coat on the aluminum support). All isolated
yields are corrected for impurities (if present).
or Fluorochem and were used without purification. Solvents were purchased
from VWR Chemicals (CH2Cl2) or Sigma-Aldrich
[toluene, dioxane, and dimethyl sulfoxide (DMSO)] and used without
purification unless stated otherwise. Dry solvents were dried over
an inert PS-MD-5 solvent purification system, equipped with an activated
alumina/copper wire column. Microwave reactions were performed in
a closed vessel in a Biotage Initiator, measuring temperature by IR. 1H NMR measurements were acquired on a Bruker AVANCE 300 (300.13
MHz) or Bruker AVANCE 500 (500.23 MHz) spectrometer. 13C NMR measurements were acquired on a Bruker AVANCE 500 (125.78 MHz)
spectrometer. Chemical shifts are reported in parts per million downfield
of tetramethylsilane and are corrected according to the solvent. Mass
analysis was performed using a Bruker MicrOTOF-Q instrument on a positive
ion polarity mode for ESI (electrospray ionization). Capillary charge:
4000 V. Melting points were measured using a Büchi M-565 melting
point apparatus. SiO2 column chromatography was performed
using Merck silica gel C60 (particle size 40–60 μm).
Thin-layer chromatography (TLC) was performed on Merck silica gel
C60 F254 plates (silica coat on the aluminum support). All isolated
yields are corrected for impurities (if present).
6
Characterization of deprotonated 4B products
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HRMS of the negatively charged deprotonated products (positively charged Na-adducts of 4B ) were recorded on a Bruker Daltonics micrOTOF-Q instrument using an electrospray ionization/quadrupole/time-of-flight systems.
1H and 13C-NMR spectra were recorded on a Bruker AV 500 spectrometer at 500 and 125 MHz, respectively. 2D-experiments were recorded using standard pulse sequences, and the chemical shifts are reported downfield from tetramethylsilane.
GC-EIMS analyses were performed on an Agilent Technologies 7890A GC-system equipped with a 5975C EIMS-detector and an Agilent J&W HP-5ms GC Column (30 m × 0.25 mm, 0.25 μm film) (Agilent Technologies Inc., Santa Clara, CA, USA).
HP-SEC analyses were performed on an Agilent 1100 Series HPLC instrument equipped with a G1315B DAD-detector, 2 × Jordi Gel DVB 500A (300 mm × 7.8 mm) columns (Columnex LLC, New York, NY, USA; 40 °C), and a 50 mm × 7.8 mm guard column. One percent of AcOH in THF served as eluent at a flow rate of 0.8 mL/min.
1H and 13C-NMR spectra were recorded on a Bruker AV 500 spectrometer at 500 and 125 MHz, respectively. 2D-experiments were recorded using standard pulse sequences, and the chemical shifts are reported downfield from tetramethylsilane.
GC-EIMS analyses were performed on an Agilent Technologies 7890A GC-system equipped with a 5975C EIMS-detector and an Agilent J&W HP-5ms GC Column (30 m × 0.25 mm, 0.25 μm film) (Agilent Technologies Inc., Santa Clara, CA, USA).
HP-SEC analyses were performed on an Agilent 1100 Series HPLC instrument equipped with a G1315B DAD-detector, 2 × Jordi Gel DVB 500A (300 mm × 7.8 mm) columns (Columnex LLC, New York, NY, USA; 40 °C), and a 50 mm × 7.8 mm guard column. One percent of AcOH in THF served as eluent at a flow rate of 0.8 mL/min.
7
Comprehensive Characterization of Novel Compounds
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1H and 13C NMR spectra for compounds were obtained in DMSO-d6, using a Bruker AMX-500 NMR spectrometer. Transmission electron microscopy (TEM) images were obtained on a HITACHI H-7000 FA transmission electron microscope. High-resolution mass spectrometry (HR MS–ESI) spectra were recorded on a Bruker micro TOF-Q instrument. The magnetic properties were measured at 300 K with a vibrating sample magnetometer (SQUID-VSM, Quantum Design, American). In vitro fluorescence images of cells were recorded on a confocal laser scanning microscope (CLSM, Nikon, Japan). The surface areas were measured by an ASAP-2020 physisorption apparatus (Micromeritics, American). The UV–Vis absorption spectra were determined by an Evolution 220 spectrophotometer (Thermofisher Scientific). The size distributions and zeta potentials were measured by a Malvern Zetasizer 90. The metal contents in cells and tissues were tested by ICP-MS (FLEXAR NEXLON300X).
8
ESI-TOF MS Analysis of Samples
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The high-resolution
mass spectra of all samples were obtained by means of electrospray
ionization time-of-flight mass spectrometry (ESI-TOF MS) using a Micro
TOF-Q instrument (Bruker Daltonics, Bremen, Germany) interfaced to
a Series 1200 HPLC Agilent pump and controlled using Compass software.
ESI-L low-concentration tuning mix (Agilent Technologies, Santa Clara,
CA) was used as a calibrator. A 5:95 mixture of acetonitrile:ammonium
acetate (15 mM) was used as a running buffer for neutral (pH 7.5)
conditions. Instrument conditions were as follows: 10–45 μL
of sample solution was injected through a polyether heteroketone (PEEK)
tube (0.5–1.5 m, 0.18 mm i.d.) at 25–50 μL·min–1, applying a capillary counter-electrode voltage of
3.5–5. 5 kV, a dry temperature of 90–110 °C, dry
gas at 6 L min–1, and a spectral collection range
of 300–2000 m/z. All spectra
were processed using Bruker Data Analysis software. The metal-to-ligand
molar ratio was 1:1.
mass spectra of all samples were obtained by means of electrospray
ionization time-of-flight mass spectrometry (ESI-TOF MS) using a Micro
TOF-Q instrument (Bruker Daltonics, Bremen, Germany) interfaced to
a Series 1200 HPLC Agilent pump and controlled using Compass software.
ESI-L low-concentration tuning mix (Agilent Technologies, Santa Clara,
CA) was used as a calibrator. A 5:95 mixture of acetonitrile:ammonium
acetate (15 mM) was used as a running buffer for neutral (pH 7.5)
conditions. Instrument conditions were as follows: 10–45 μL
of sample solution was injected through a polyether heteroketone (PEEK)
tube (0.5–1.5 m, 0.18 mm i.d.) at 25–50 μL·min–1, applying a capillary counter-electrode voltage of
3.5–5. 5 kV, a dry temperature of 90–110 °C, dry
gas at 6 L min–1, and a spectral collection range
of 300–2000 m/z. All spectra
were processed using Bruker Data Analysis software. The metal-to-ligand
molar ratio was 1:1.
9
General Organic Chemistry Procedures
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Chemicals were purchased from Sigma-Aldrich
or Fluorochem and were used without purification. Solvents were purchased
from VWR Chemicals (CH2Cl2) or Sigma-Aldrich
(toluene, dioxane, DMSO) and used without purification, unless stated
otherwise. Dry solvents were dried over an inert PS-MD-5 solvent purification
system, equipped with an activated alumina/copper wire column. 1H NMR measurements were acquired on a Bruker Avance 300 (300.13
MHz) or Bruker Avance 500 (500.23 MHz) spectrometer. 13C NMR measurements were acquired on a Bruker Avance 500 (125.78 MHz)
spectrometer. Chemical shifts are reported in parts per million downfield
of tetramethylsilane and are corrected according to solvent. Mass
analysis was performed using a Bruker MicrOTOF-Q instrument on a positive
ion polarity mode for ESI (electrospray ionization). Capillary charge:
4000 V. Melting points were measured using a Büchi M-565 melting
point apparatus. SiO2 column chromatography was performed
using Merck silica gel C60 (particle size 40–60 μm).
TLC chromatography was performed on Merck silica gel C60 F254 plates
(silica coat on aluminum support). All isolated yields are corrected
for present impurities (if present).
or Fluorochem and were used without purification. Solvents were purchased
from VWR Chemicals (CH2Cl2) or Sigma-Aldrich
(toluene, dioxane, DMSO) and used without purification, unless stated
otherwise. Dry solvents were dried over an inert PS-MD-5 solvent purification
system, equipped with an activated alumina/copper wire column. 1H NMR measurements were acquired on a Bruker Avance 300 (300.13
MHz) or Bruker Avance 500 (500.23 MHz) spectrometer. 13C NMR measurements were acquired on a Bruker Avance 500 (125.78 MHz)
spectrometer. Chemical shifts are reported in parts per million downfield
of tetramethylsilane and are corrected according to solvent. Mass
analysis was performed using a Bruker MicrOTOF-Q instrument on a positive
ion polarity mode for ESI (electrospray ionization). Capillary charge:
4000 V. Melting points were measured using a Büchi M-565 melting
point apparatus. SiO2 column chromatography was performed
using Merck silica gel C60 (particle size 40–60 μm).
TLC chromatography was performed on Merck silica gel C60 F254 plates
(silica coat on aluminum support). All isolated yields are corrected
for present impurities (if present).
10
Analytical Characterization of Organic Compounds
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Commercially available reagents and solvents were of analytical grade or were purified by standard procedures prior to use. Reactions were monitored via thin-layer chromatography (TLC). The 1H NMR and 13C NMR spectra were recorded on a 200(50) MHz and 400(100) MHz Varian spectrometer using CDCl3. Chemical shifts (δ) are reported in parts per million (ppm) relative to either a tetramethylsilane (TMS) internal standard or solvent signals. Interchangeable hydrogens and carbons were assigned with the letter. High-resolution mass spectrometry (HRMS) were recorded in Bruker Daltonics microTOF-Q instrument by using atmospheric pressure chemical ionization-electrospray ionization (APCI-ESI) ion source. Column chromatography was performed on silica gel 60 (70–230 mesh ASTM), and TLC was carried out on silica gel (254–366 mesh ASTM). The purity of biologically tested compounds was determined by Q NMR (purity >98%)20–23 (link).
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