All chemicals and solvents were of commercial reagent quality and were used without further purification unless otherwise stated. DMA was dried over molecular sieves of size 4 Å and distilled under reduced pressure. TEOA was distilled under reduced pressure. Tetraethylammonium tetrafluoroborate was dried in vacuo at 100°C overnight before use. [Ir(piq)2(BL)](PF6) (Kuramochi and Ishitani, 2016 (link)), BNAH (Mauzerall and Westheimer, 1955 (link)), BI(OH)H (Hasegawa et al., 2005 (link); Zhu et al., 2008 (link)), Ru (Anderson et al., 1995 (link)), and BL (Sun et al., 1997 (link)) were synthesized according to literature procedures. 1H NMR spectra were recorded on an AL400 NMR spectrometer. IR spectra were measured in dichloromethane on a JASCO FT/IR-610 spectrometer. Electrospray ionization–mass spectroscopy (ESI-MS) was undertaken using a SHIMADZU LCMS-2010A system with acetonitrile as a mobile phase. UV–vis absorption spectra were recorded with a JASCO V-670 instrument. Emission spectra were measured at 25°C under an Ar atmosphere using a JASCO FP-8600 spectrofluorometer with correlation for the detector sensitivity. Emission quenching experiments were performed in DMA or DMA/TEOA (5:1 v/v) solutions containing a complex and several different concentrations of BNAH or BI(OH)H.
Lcms 2010a system
Manufactured by Shimadzu
Sourced in Japan
The LCMS-2010A is a liquid chromatography-mass spectrometry (LC-MS) system manufactured by Shimadzu. It is designed to perform sensitive and accurate analysis of a wide range of compounds. The system combines a high-performance liquid chromatograph (HPLC) with a single quadrupole mass spectrometer, enabling the separation, identification, and quantification of various analytes in complex samples.
Automatically generated - may contain errors
Lab products found in correlation
Ftir 610, by Jasco (2 mentions)
Fp 8600 spectrofluorometer, by Jasco (1 mentions)
Ft ir 610 spectrometer, by Jasco (1 mentions)
V 670 instrument, by Jasco (1 mentions)
Eca400 2, by JEOL (1 mentions)
Ft ir 6600 spectrometer, by Jasco (1 mentions)
Highly polymerized calf thymus dna, by Merck Group (1 mentions)
460 plus ftir spectrophotometer, by Jasco (1 mentions)
Mpf 4 spectrofluorimeter, by Hitachi (1 mentions)
Lc ms 2010a, by Shimadzu (1 mentions)
6 protocols using lcms 2010a system
1
Synthesis and Characterization of Photocatalysts
2
Detailed Spectroscopic Characterization
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FT-IR spectra were measured using a JASCO FT/IR-610 or 6600 spectrometer at 1 cm–1 resolution. 1H NMR and 13C NMR spectra were measured in acetonitrile-d3, DMF-d7 or DMSO-d6 using a JEOL ECA400-II at 400 and 100 MHz, respectively. Electrospray ionisation mass spectroscopy (ESI-MS) was performed using a Shimadzu LCMS-2010A system with acetonitrile as the mobile phase.
3
Characterization of Rhenium Complexes
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1H NMR spectra were recorded in CDCl3 or CD3CN on a JEOL ECA400-II system at 400 MHz. Transmission IR spectra in CH2Cl2 or the reaction solution were recorded on a JASCO FT/IR-610 or FT/IR-6600 spectrometer at 1 cm–1. Electrospray ionization-mass spectroscopy (ESI-MS) was performed using a Shimadzu LC-MS-2010 A system with MeCN as the mobile phase. Solutions containing 5 mM complexes and 0.1 M Et4NBF4 were prepared for the FT-IR measurements, and a solution containing only 0.1 M Et4NBF4 was used for the background measurements. Ultra high performance chromatograms (UHPLC) of the Re complexes were recorded on a SHIMADZU UHPLC Nexera X2 with an ODS column (Waters Acquity: 150 mm × 2.1 mm i.d.), a Shimadzu DGU-20A degasser, an LC-30AD pump, an SPD-M30A UV-vis photodiode-array detector, and a Rheodyne 7125 injector. The eluent was a 1 : 1 (v/v) mixture of methanol and water containing 0.05 M KH2PO4 (pH 5.9), and the flow rate was 0.2 mL min–1.
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1H NMR spectra were recorded in CDCl3 or CD3CN on a JEOL ECA400-II system at 400 MHz. Transmission IR spectra in CH2Cl2 or the reaction solution were recorded on a JASCO FT/IR-610 or FT/IR-6600 spectrometer at 1 cm–1. Electrospray ionization-mass spectroscopy (ESI-MS) was performed using a Shimadzu LC-MS-2010 A system with MeCN as the mobile phase. Solutions containing 5 mM complexes and 0.1 M Et4NBF4 were prepared for the FT-IR measurements, and a solution containing only 0.1 M Et4NBF4 was used for the background measurements. Ultra high performance chromatograms (UHPLC) of the Re complexes were recorded on a SHIMADZU UHPLC Nexera X2 with an ODS column (Waters Acquity: 150 mm × 2.1 mm i.d.), a Shimadzu DGU-20A degasser, an LC-30AD pump, an SPD-M30A UV-vis photodiode-array detector, and a Rheodyne 7125 injector. The eluent was a 1 : 1 (v/v) mixture of methanol and water containing 0.05 M KH2PO4 (pH 5.9), and the flow rate was 0.2 mL min–1.
4
Characterization of Pt(II) Complexes
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Highly polymerized calf thymus
DNA was purchased from Sigma-Aldrich. All chemicals and solvents were
prepared by Merck (Germany). cis-[Pt(NH3)2I2] and [Pt(bipy)Cl2] were synthesized
using the methods described in the literature.52 (link)−55 (link) Infrared monitoring (4000–400
cm–1) was done on a JASCO-460 plus FT-IR spectrophotometer.
LC-MS analysis was performed on a Shimadzu LC-MS-2010 A system. A
Bruker BRX-250 Avance spectrometer was used at 300, 75, and 64 MHz
for 1H NMR, 13C NMR, and 195Pt NMR
monitoring, respectively. A Systronics Conductivity Bridge, model
305 (cell constant of 0.59), was used to measure the conductivities
of the two complexes in water. Melting points were recorded using
a Buchi B-545 system. A circular dichroism study was done using a
Jasco J-1500 CD spectrometer. The absorbance was recorded using a
SPEKOL 2000 UV 6800 spectrophotometer. The fluorescence intensity
was examined using a Hitachi MPF-4 spectrofluorimeter.
DNA was purchased from Sigma-Aldrich. All chemicals and solvents were
prepared by Merck (Germany). cis-[Pt(NH3)2I2] and [Pt(bipy)Cl2] were synthesized
using the methods described in the literature.52 (link)−55 (link) Infrared monitoring (4000–400
cm–1) was done on a JASCO-460 plus FT-IR spectrophotometer.
LC-MS analysis was performed on a Shimadzu LC-MS-2010 A system. A
Bruker BRX-250 Avance spectrometer was used at 300, 75, and 64 MHz
for 1H NMR, 13C NMR, and 195Pt NMR
monitoring, respectively. A Systronics Conductivity Bridge, model
305 (cell constant of 0.59), was used to measure the conductivities
of the two complexes in water. Melting points were recorded using
a Buchi B-545 system. A circular dichroism study was done using a
Jasco J-1500 CD spectrometer. The absorbance was recorded using a
SPEKOL 2000 UV 6800 spectrophotometer. The fluorescence intensity
was examined using a Hitachi MPF-4 spectrofluorimeter.
5
HAMA Pigment Analysis by LC-MS
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The pigment HAMA that accumulated in verA disruptant was analyzed by liquid chromatography-mass spectrometry (LC-MS) using three conditions as follows:
Condition [A]: HPLC condition column: YMC-UltraH Pro C18 (2.0 mm I.D. × 50; YMC America, Allentown, PA, USA), solvent A: 0.1% formic acid in water, solvent B: 0.1% formic acid in CH3CN; gradient: 0 min 10% B, 2 min 10% B, 10 min 100% B, 13 min 100% B, 15 min 10% B; Detection: DAD 220–340 nm MaxPlot; MS + ESI (m/z 100–1000), −ESI (m/z 100–1000).
Condition [B]: The LC-MS 2010A system (Shimadzu, Kyoto, Japan) consisted of an LC-VP separation module equipped with an SPD-M10AVp photodiode array (PDA) detector and a single-quadrupole mass spectrometer with an atmospheric pressure photoionization (APPI) source probe. Solvent A, 5 mM ammonium acetate in water; solvent B, methanol; gradient: 0 min 10%, 2 min 10%, 17 min 95%, 22 min 95%, 23 min 10%, and 30 min 10%. MS + APPI (m/z 100–500), −APPI (m/z 100–500) An Inertsil column (150 mm × 2.1 mm, 5 mm, Supelco, Bellefonte, PA, USA) was used, and the flow rate was 0.2 mL min−1.
Condition [C]: the LC-MS conditions were the same as those in condition [B] except that the carrier solvent was set as an isocratic mixture of methanol and 5 mM ammonium acetate in water (40:60, v/v).
Condition [A]: HPLC condition column: YMC-UltraH Pro C18 (2.0 mm I.D. × 50; YMC America, Allentown, PA, USA), solvent A: 0.1% formic acid in water, solvent B: 0.1% formic acid in CH3CN; gradient: 0 min 10% B, 2 min 10% B, 10 min 100% B, 13 min 100% B, 15 min 10% B; Detection: DAD 220–340 nm MaxPlot; MS + ESI (m/z 100–1000), −ESI (m/z 100–1000).
Condition [B]: The LC-MS 2010A system (Shimadzu, Kyoto, Japan) consisted of an LC-VP separation module equipped with an SPD-M10AVp photodiode array (PDA) detector and a single-quadrupole mass spectrometer with an atmospheric pressure photoionization (APPI) source probe. Solvent A, 5 mM ammonium acetate in water; solvent B, methanol; gradient: 0 min 10%, 2 min 10%, 17 min 95%, 22 min 95%, 23 min 10%, and 30 min 10%. MS + APPI (m/z 100–500), −APPI (m/z 100–500) An Inertsil column (150 mm × 2.1 mm, 5 mm, Supelco, Bellefonte, PA, USA) was used, and the flow rate was 0.2 mL min−1.
Condition [C]: the LC-MS conditions were the same as those in condition [B] except that the carrier solvent was set as an isocratic mixture of methanol and 5 mM ammonium acetate in water (40:60, v/v).
6
Phytochemical Analysis of A. euchroma
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Liquid Chromatography-Mass Spectrometry (LC-MS) Analysis.
LC-MS studies of the different extracts of A. euchroma were performed applying a Shimadzu LCMS 2010 ASystem consisting of a degasser, binary pump, autosampler, and column heater. The column outlet was coupled to a Thermo fleet (LCQ-Fleet) Ion Trap mass spectrometer equipped with an ESI ion source. Data acquisition and mass spectrometric assessments were performed in a personal computer with Data Analysis software (Shimadzu LC-MS 2010 A). To chromatographic separation, a Phenomenex luna 5-µm C8 column (4.6 × 250 mm) was employed. The column was kept at 95% Solvent A (Acetonitrile 0.1% Formic Acid) and 5% Solvent B (H_2 O 0.1% Formic Acid) for 1 min, followed by an 11 min step gradient from 5% B to 100% B, next it was held for 4 min with 100% B. Ultimately, elution was performed with a linear gradient from 100% B to 5% B for 2 min. The flow rate was set at 0.25 ml/min and also the injection volume 5 µl. The following parameters were applied during the MS test: to electrospray ionization with positive ion polarity, the capillary voltage was set to 30 V, the capillary temperature to 280°C, the nebulizer pressure to 40 psi, and the drying gas flow rate to 1.2 L/ min.
LC-MS studies of the different extracts of A. euchroma were performed applying a Shimadzu LCMS 2010 ASystem consisting of a degasser, binary pump, autosampler, and column heater. The column outlet was coupled to a Thermo fleet (LCQ-Fleet) Ion Trap mass spectrometer equipped with an ESI ion source. Data acquisition and mass spectrometric assessments were performed in a personal computer with Data Analysis software (Shimadzu LC-MS 2010 A). To chromatographic separation, a Phenomenex luna 5-µm C8 column (4.6 × 250 mm) was employed. The column was kept at 95% Solvent A (Acetonitrile 0.1% Formic Acid) and 5% Solvent B (H_2 O 0.1% Formic Acid) for 1 min, followed by an 11 min step gradient from 5% B to 100% B, next it was held for 4 min with 100% B. Ultimately, elution was performed with a linear gradient from 100% B to 5% B for 2 min. The flow rate was set at 0.25 ml/min and also the injection volume 5 µl. The following parameters were applied during the MS test: to electrospray ionization with positive ion polarity, the capillary voltage was set to 30 V, the capillary temperature to 280°C, the nebulizer pressure to 40 psi, and the drying gas flow rate to 1.2 L/ min.
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