Optical rotations were recorded on a Jasco DIP-370 polarimeter. The 1D (1H and 13C) and 2D (HSQC, HMBC, 1H-1H COSY, and NOESY) NMR experiments were recorded on a Bruker DRX 600 NMR spectrometer (Bruker, Billerica, MA, USA). HR-ESI-MS and HR-FAB-MS were measured on an LC-MS-Q-TOF (Agilent Tokyo, Japan) and a JMS-700 mass spectrometer (JEOL, Tokyo, Japan), respectively. Coupling constants are expressed in Hz, and chemical shifts in δ (ppm). Chromatographic separations were performed using column chromatography on a Merck silica gel (70–230), and Medium-Pressure Liquid Chromatography (MPLC) (Büchi Reveleris® Prep system, Flawil, Switzerland) was performed using a silica gel cartridge (40 μM, 12 g) and a C-18 cartridge (WP, 20 μM, 4 g) with a UV-ELSD detector. Thin-layer chromatography (TLC) was performed on glass pre-coated silica gel 60 F254 plates (Merck, Darmstadt, Germany) and reversed phase (RP-18 F254), which were visualized under UV light at (254 and 365 nm) and sprayed with 5% MeOH-H2SO4 reagent, followed by heating for 2–3 min.
Lc ms q tof
Manufactured by Agilent Technologies
Sourced in United States
The LC-MS-Q-TOF is a laboratory instrument that combines liquid chromatography (LC) with quadrupole time-of-flight mass spectrometry (Q-TOF). It is designed to perform high-resolution, accurate-mass analysis of molecular compounds.
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Lab products found in correlation
Jms 700 mass spectrometer, by JEOL (1 mentions)
Dip 370 polarimeter, by Jasco (1 mentions)
Drx 600 nmr spectrometer, by Bruker (1 mentions)
1260 infinity series hplc, by Agilent Technologies (1 mentions)
Ascentis express c18 column, by Merck Group (1 mentions)
Eclipse plus c18 column, by Agilent Technologies (1 mentions)
Agilent masshunter qualitative analysis b 05, by Agilent Technologies (1 mentions)
4 protocols using lc ms q tof
1
Spectroscopic Characterization of Organic Compounds
2
Spectrometric Analysis of Plant Extracts
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Following the method described by Marra et al. [73 (link)], the spectrometric analysis of the plant extracts was performed by an LC-MS Q-TOF Agilent Technologies (Santa Clara, CA, USA), equipped with a 1260 Infinity series HPLC with DAD detector, and a mass spectrometer Q-TOF (model G6540) with Dual ESI source. The plant extracts were separated with a reverse-phase analytical Ascentis ® Express C18 column (2.7 μm, 50 mm × 3.0 mm id, Supelco ©, Bellefonte, PA, USA). The identification and quantification of the three phenolic acids p-coumaric, caffeic and rosmarinic were obtained by comparing the mass and the retention time (RT) to standard compounds (Sigma-Aldrich, St. Louis, MO, USA). These standards were analyzed with the same LC-MS method and the quantification was obtained by interpolating the averaged data with a previously constructed calibration curve.
3
Comprehensive LCMS Analysis of FPH
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Characteristic components of FPH were analyzed by Agilent LC/MS Q-TOF (USA, 1290-6545). The UPLC chromatographic conditions were ZORBAX Eclipse Plus C18 column (3.0 mm × 150 mm, 1.8 μm), 30°C of column temperature, and mixed mobile phase (phase A: 0.1% of formic acid in water, mobile phase B: 100% acetonitrile) with a gradient elution program (5% B (0-2 min), 5% B → 35% B (2-20 min), 35% B → 50% B (20-24 min), 50% B → 40% B (24-25 min), 40% B → 95% B (25-30 min), and 95% B (30-35 min)) at 0.5 mL/min of flow rate and 0.5 μL of injection volume. The mass spectrometer was the Agilent G6545 quadruple-time-of-flight spectrometer coupled with an Agilent Jet Stream Electrospray source (Agilent, CA, USA). The system was operated in positive or negative scan modes. The instrument parameters were 3500 kV (-) or 4000 V(+) of capillary voltage, N2 drying gas with 11 L/min of flow rate at 300°C temperature, 350°C of sheath gas temperature, 130 V of cataclastic voltage, 45 psi of nebulizer pressure, MS scan and m/z 100–1000, and 8 spectrums of the scan speed.
4
Phytochemical Analysis of M. porteri Extract
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Gummy texture of M. porteri's ethanolic extract (10 mg) was obtained from the drying process using a rotary evaporator. 1 mL of methanol was used to dilute the gummy extract to a final concentration of 10 mg/mL. Then, the extract was diluted again with methanol to a concentration of 1 mg/mL. The extract was filtered with a 0.22 μm pore size syringe filter before performing the analysis using LC-MS/QTOF (model 6520 Agilent Technologies, SA, USA). 2 μl of the filtered extract was injected into Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HT column (2.1 mm × 100 mm × 1.8 μm, Agilent Technologies, SA, USA) at the temperature of 40 °C. The flow rate used was 0.25 mL/min with solvent A (0.1% formic acid in distilled water) and solvent B (0.1% formic acid in acetonitrile). The gradient elution program was 0.00–18.00 min for 5–95% of mobile phase (B), 18–23 min for 95% of mobile phase (B) and 23.01 min for 5% of mobile phase (B). The total run time for analysis of the extract was 30 min. The mass spectrometer was set to positive electrospray ionisation (ESI) mode with an optimal gas temperature of 325 °C, gas flow of 11 L/min, and nebulizer pressure of 35 psi. The Agilent Mass Hunter Qualitative Analysis B.05.00 software (Agilent Technologies, Santa Clara, CA, USA) was used to analyze the MS data and METLIN database was used to annotate the predicted chemical compounds [25 (link)].
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