The crude extracts were dissolved in ACN-H2O (8:2) and assessed by HPLC-DAD and UPLC-DAD-QTOF using modified chromatographic conditions from literature28 (link). For UPLC-DAD-QTOF, samples were ionized by ESI with a MicrOTOF Bruker Daltonics mass spectrometer (Milford MA, USA). Mass spectra were obtained in positive ionization mode and the following parameters were applied: capillary energy of 3.5 kV, nitrogen was used as nebulization, drying gas (5.5 bar and 10 L/h), and temperature drying time of 220 °C. UPLC conditions were carried out using the isocratic system: 0–18′ (60:40; A:B), 18–32′ (50:50; A:B), and 32–40′ (100% of B %), 0.3 mL.min−1 flow rate and detection at 245 nm (A-triethylammonium acetate buffer 35 mM, 0.2% v/v, pH 6.9; B-ACN); and an Agilent Zorbax Eclipse XDB-C18 column: 3.5 µ, 4.6 × 150 mm. For HPLC-DAD, the samples were analyzed with the same chromatographic conditions described above, except for the flow rate, which was 0.8 mL.min−1.
Microtof daltonics mass spectrometer
Manufactured by Bruker
Sourced in United States
The MicrOTOF Bruker Daltonics mass spectrometer is a high-resolution time-of-flight mass spectrometer. It is designed to provide accurate mass measurements for a wide range of analytes.
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2 protocols using microtof daltonics mass spectrometer
1
Comprehensive Analysis of Crude Extracts
2
Inert Atmosphere Organic Synthesis
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Materials Reactions were performed in oven-dried glassware and magnetically stirred under an inert atmosphere using a syringe tube equipped with an argon or nitrogen balloon.
Room temperature was 25°C. Commercial solvents and reagents were used as received. Anhydrous solvents were dried over 4 Å molecular sieves. All reactions were monitored by TLC using aluminium silica gel 60 F254 (Merck). IR spectra were measured on a Fourier transform (FT)-IR spectrometer, Per kinElmer, Inc. (U.S.A.) 1 H-and 13 (link) C-NMR spectra were obtained on a Bruker Avance DPX-300 FT-NMR spectrometer. 1 (link) H-NMR chemical shifts (δ) and coupling constants (J) were given in ppm and Hz, respectively. Deuterated chloroform (CDCl 3 ) served as an internal standard for both 1 H-and 13 C-NMR spectra at 7.26 and 77.0 ppm, respectively. Mass spectra were recorded on a microTOF Bruker Daltonics mass spectrometer.
Room temperature was 25°C. Commercial solvents and reagents were used as received. Anhydrous solvents were dried over 4 Å molecular sieves. All reactions were monitored by TLC using aluminium silica gel 60 F254 (Merck). IR spectra were measured on a Fourier transform (FT)-IR spectrometer, Per kinElmer, Inc. (U.S.A.) 1 H-and 13 (link) C-NMR spectra were obtained on a Bruker Avance DPX-300 FT-NMR spectrometer. 1 (link) H-NMR chemical shifts (δ) and coupling constants (J) were given in ppm and Hz, respectively. Deuterated chloroform (CDCl 3 ) served as an internal standard for both 1 H-and 13 C-NMR spectra at 7.26 and 77.0 ppm, respectively. Mass spectra were recorded on a microTOF Bruker Daltonics mass spectrometer.
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