L. shawii metabolites were separated and tentatively identified using an Agilent (Santa Clara, CA) 1,260 Infinity high-performance liquid chromatography (LC) system coupled to an Agilent 6,530 quadrupole time-of-flight (QTOF), as described in Alehaideb et al. (2022) (link). Briefly, the separation was performed on an Agilent SB-C18 column (4.6 mm × 150 mm, 1.8 μm particle size) with the gradient elution: 0–2 min, 5% B; 2–17 min, 5%–100% B; 17–21 min, 95% B; 21–25 min, 5% B, using mobile-phase A (0.1% formic acid in water) and mobile-phase B (0.1% formic acid in methanol). The injection volume was 10 μL, and the flow rate was 250 μL/min. The gas temperature was set at 300°C, the gas flow at 8 L/min, the nebulizer pressure at 35 psi, the sheath gas flow rate at 11 L/min, the gas temperature at 350°C, and the scanning range was set from 50 to 800 (m/z). The data were generated by the Agilent MassHunter (version B.06.00) analysis software.
6 530 quadrupole time of flight
Manufactured by Agilent Technologies
Sourced in Canada, United States
The 6,530 quadrupole time-of-flight is a high-performance mass spectrometry instrument designed for accurate mass measurements and structural analysis. It combines a quadrupole mass analyzer with a time-of-flight mass analyzer to provide high resolving power and mass accuracy.
Automatically generated - may contain errors
Lab products found in correlation
Sb c18 column, by Agilent Technologies (2 mentions)
1260 infinity high, by Agilent Technologies (1 mentions)
0.25 mm silica gel plates, by Merck Group (1 mentions)
Silica gel 60, by Merck Group (1 mentions)
Agilent 1260 infinity hplc system, by Agilent Technologies (1 mentions)
1260 infinity hplc system, by Agilent Technologies (1 mentions)
4 protocols using 6 530 quadrupole time of flight
1
Metabolite Profiling of Leishmania shawii
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L. shawii metabolites were separated and tentatively identified using an Agilent (Santa Clara, CA) 1,260 Infinity high-performance liquid chromatography (LC) system coupled to an Agilent 6,530 quadrupole time-of-flight (QTOF), as described in Alehaideb et al. (2022) (link). Briefly, the separation was performed on an Agilent SB-C18 column (4.6 mm × 150 mm, 1.8 μm particle size) with the gradient elution: 0–2 min, 5% B; 2–17 min, 5%–100% B; 17–21 min, 95% B; 21–25 min, 5% B, using mobile-phase A (0.1% formic acid in water) and mobile-phase B (0.1% formic acid in methanol). The injection volume was 10 μL, and the flow rate was 250 μL/min. The gas temperature was set at 300°C, the gas flow at 8 L/min, the nebulizer pressure at 35 psi, the sheath gas flow rate at 11 L/min, the gas temperature at 350°C, and the scanning range was set from 50 to 800 (m/z). The data were generated by the Agilent MassHunter (version B.06.00) analysis software.
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L. shawii metabolites were separated and tentatively identified using an Agilent (Santa Clara, CA) 1,260 Infinity high-performance liquid chromatography (LC) system coupled to an Agilent 6,530 quadrupole time-of-flight (QTOF), as described in Alehaideb et al. (2022) (link). Briefly, the separation was performed on an Agilent SB-C18 column (4.6 mm × 150 mm, 1.8 μm particle size) with the gradient elution: 0–2 min, 5% B; 2–17 min, 5%–100% B; 17–21 min, 95% B; 21–25 min, 5% B, using mobile-phase A (0.1% formic acid in water) and mobile-phase B (0.1% formic acid in methanol). The injection volume was 10 μL, and the flow rate was 250 μL/min. The gas temperature was set at 300°C, the gas flow at 8 L/min, the nebulizer pressure at 35 psi, the sheath gas flow rate at 11 L/min, the gas temperature at 350°C, and the scanning range was set from 50 to 800 (m/z). The data were generated by the Agilent MassHunter (version B.06.00) analysis software.
2
Analytical Procedures for Organic Synthesis
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All starting materials and reagents
were obtained from commercial
sources and used without further purification. Air- and moisture-sensitive
reactions were performed under nitrogen. Flash column chromatography
was performed using silica gel 60 (230–400 mesh, Merck) with
the indicated solvents. Thin-layer chromatography (TLC) was performed
using 0.25 mm silica gel plates (Merck). 1H and 13C{1H} NMR spectra were recorded on a Bruker 600 MHz spectrometer
as solutions in deuterochloroform (CDCl3) or methanol-d4 (CD3OD). 1H NMR data
were reported on the order of chemical shift, multiplicity (s, singlet;
d, doublet; t, triplet; q, quartet; m, multiplet and/or multiplet
resonances), number of protons, and coupling constant (J value) in hertz (Hz). Enantiomeric excesses were determined by high-performance
liquid chromatography (HPLC) on an Agilent 1100 using one chiral column
(CHIRALPAK IA, IB, IC, ID, IG). High-resolution mass spectra (HRMS)
were recorded on an Agilent 6530 quadrupole time-of-flight (Q-TOF)
liquid chromatography (LC)/tandem mass spectrometry (MS/MS) system
(electrospray ionization (ESI)).
were obtained from commercial
sources and used without further purification. Air- and moisture-sensitive
reactions were performed under nitrogen. Flash column chromatography
was performed using silica gel 60 (230–400 mesh, Merck) with
the indicated solvents. Thin-layer chromatography (TLC) was performed
using 0.25 mm silica gel plates (Merck). 1H and 13C{1H} NMR spectra were recorded on a Bruker 600 MHz spectrometer
as solutions in deuterochloroform (CDCl3) or methanol-d4 (CD3OD). 1H NMR data
were reported on the order of chemical shift, multiplicity (s, singlet;
d, doublet; t, triplet; q, quartet; m, multiplet and/or multiplet
resonances), number of protons, and coupling constant (J value) in hertz (Hz). Enantiomeric excesses were determined by high-performance
liquid chromatography (HPLC) on an Agilent 1100 using one chiral column
(CHIRALPAK IA, IB, IC, ID, IG). High-resolution mass spectra (HRMS)
were recorded on an Agilent 6530 quadrupole time-of-flight (Q-TOF)
liquid chromatography (LC)/tandem mass spectrometry (MS/MS) system
(electrospray ionization (ESI)).
3
HPLC-QTOF Analysis of Compounds
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Extract analysis was performed by the Agilent1260 Infinity HPLC system combined with Agilent 6530 quadrupole time of flight (Markham, ON, Canada). Agilent extend-C18 column (2.1 mm × 50 mm, 1.8 μm) was used for separation, applying the same elution gradient for RP- HPLC analysis. A volume of 10 µL was inserted at a flow rate of 300 µL/min. The MS1 acquisition technique was attained at 100–600 m/z mass in positive mode. The mass spectrometer was set at 300 °C, and 8 L/min as gas temperature and gas flow rate, respectively; 35 psig for Nebulizer; 350 °C and 1 L were SheathGas temperature and SheathGas flow rate, respectively. Agilent MassHunter, qualitative analysis software (Wilmington, DE, USA) was used for MS1 data.
4
Identification of A. fragrantissima Flower Metabolites
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The method of separation and identification of A. fragrantissima flower metabolites in dichloromethane extract was performed using an Agilent (Santa Clara, CA, USA) 1260 Infinity HPLC system coupled to Agilent 6530 quadrupole time-of-flight (Q-TOF) as described earlier in [69 (link)]. Briefly, the separation was performed using an Agilent SB-C18 column (4.6 mm × 150 mm, 1.8 μm) with the following elution gradient; 0 to 2 min, 5% B; 2 to 17 min, 5 to 100% B; 17 to 21 min, 95% B; 21 to 25 min, 5% B, using mobile-phase A (0.1% formic acid in water) and mobile-phase B (0.1% formic acid in methanol). The flow rate was set at 250 μL/min and injection volume was 10 μL. The scanning range was set at 50–800 (m/z), gas temperature at 300 °C gas flow of 8 L/min, nebulizer pressure of 35 psi, sheath gas temperature at 350 °C, and sheath gas flow rate of 11 L/min. The data were generated by the Agilent MassHunter (version B. 06.00) qualitative analysis software.
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