All NMR spectra were obtained on a Bruker Avance DPX400 spectrometer at 400 MHz for 1H-NMR or 100 MHz for 13C-NMR. The quantitative analysis was performed using an Agilent 1100 LC/MSD VL system (G1946C) (Agilent Technologies, Palo Alto, CA, USA) The LC-ESI-MS determination was performed by operating the MSD in the positive or negative ion mode. Spectra were acquired over the scan range 50–1500 m/z using a step size of 0.1 u. Chromatographic analysis was performed using a Varian Polaris 5 C18-A column (150 × 4.6 mm, 5 µm particle size) at rt. Analysis was carried out using a gradient elution of a binary solution; eluent A was ACN, while eluent B consisted of water. The analysis started at 0% A for three minutes; then, it rapidly increased up to 98% in 12 min and finally remained at 98% A until 18 min. The analysis was performed at a flow rate of 0.8 mL min−1, and the injection volume was 20 µL. The purity of compounds (as measured by peak area ratio) was >97%.
Agilent 1100 lc msd vl system
Manufactured by Agilent Technologies
Sourced in United States
The Agilent 1100 LC/MSD VL system is a liquid chromatography-mass spectrometry (LC/MS) instrument designed for qualitative and quantitative analysis of compounds in various sample matrices. It combines high-performance liquid chromatography (HPLC) with a single quadrupole mass spectrometer, providing accurate mass detection and identification capabilities.
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Lab products found in correlation
6 protocols using agilent 1100 lc msd vl system
1
Quantitative Analysis of Compounds by LC-ESI-MS
2
LC-MS Quantification of Organic Compounds
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UV/LC–MS chromatographic analyses were carried out using an Agilent 1100 LC/MSD VL system (G1946C) purchased from Agilent Technologies (Palo Alto, CA, USA). Chromatographic separations were achieved at room temperature (RT) using a Phenomenex Kinetex C18-100 column (150 mm × 4.6 mm, 5 µm) and gradient elution consisting of a solution of solvent A (H2O) and solvent B (ACN), both acidified with 0.1% v/v formic acid (FA). The analysis began with 5% B (t = 0–1 min), increased to 95% (t = 1–10 min), maintained at 95% (t = 10–19 min), and finally returned to 5% solvent A. The analyses were performed at a flow rate of 0.6 mL/min, UV detection was monitored at 254 nm, and spectra were acquired over the scan range of m/z 100–1000 in both positive and negative modes.
3
Synthesis and Characterization of Organic Compounds
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All commercially available chemicals and solvents were used as purchased. THF was dried over sodium and benzophenone prior to use. Anhydrous reactions were run under positive pressure of dry nitrogen. TLC was carried out using Merck TLC plates silica gel 60 F254 (Merck, Kenilworth, NJ). 1H NMR and 13C NMR were recorded at 400 and 100 MHz, respectively, on a Bruker AC200F spectrometer (Bruker, Billerica, MA). Proton shift for 1H NMR are reported in parts per million (δ scale) and internally referenced to the CDCl3 or DMSO signal, at 7.26 and 2.50 ppm, respectively. Chemical shifts for carbon are reported in parts per million (δ scale) and referenced to the carbon resonances of the solvent (CDCl3 at δ 77.16 and DMSO at δ 39.52 ppm). Data are shown as following: chemical shift, multiplicity (s = singlet, d = doublet, t = triplet, m = multiplet, and/or multiplet resonances), coupling constant (J) in Hertz (Hz), and integration. Mass spectra (MS) data were obtained using an Agilent 1100 LC/MSD VL system (G1946C) (Agilent Technologies, Palo Alto, CA) by direct injection with a 0.4 ml min−1 flow rate using a binary solvent system of MeOH:H2O (95:5). UV detection was monitored at 254 nm. MS were acquired in positive scanning mode over the mass range m/z 50–1500.
4
LC-UV/MS Analysis of Compounds
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LC chromatographic analyses were performed by UV/LC-MS with an Agilent 1100 LC/MSD VL system (G1946C) (Agilent Technologies, Palo Alto, CA) equipped with a vacuum solvent degassing unit, a binary high-pressure gradient pump, an 1100 series UV detector, and a 1100 MSD model VL benchtop mass spectrometer. Chromatographic separations were obtained using a Phenomenex Kinetex C18-100 Å column (150 × 4.6 mm) with 5 µm particle size and gradient elution with a binary solution; (eluent A: H2O acidified with formic acid (FA) 0.1% v/v, eluent B: ACN/MeOH 1:1 v/v) at room temperature. The analysis started with 5% of B (from t = 0 to t = 1 min), then B was increased to 95% (from t = 1 to t = 10 min), then kept at 95% (from t = 10 to t = 15 min) and finally returned to 5% of eluent A in one minute. The instrument worked in positive mode and the UV detector operated at 254 nm.
5
Artemisinin Derivative Synthesis and Characterization
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All reactions were performed
in flame-dried glassware under a nitrogen atmosphere. Reagents were
obtained from commercial suppliers (Sigma-Aldrich Srl, Milan, Italy)
and used without further purification. TLC chromatography was performed
on precoated aluminum silica gel SIL G/UV254 plates (Macherey-Nagel
& Co.). The detection occurred via fluorescence quenching or development
in a molybdato phosphate solution (10% in EtOH). Merck silica gel
60 was used for flash chromatography (23–400 mesh). All products
were dried in high vacuum (10-3 mbar). 1H NMR and 13C NMR spectra were measured on a Bruker Avance
DRX400 (400 MHz/100 MHz) and on a Bruker Avance DPX200 (200 MHz/50
MHz) spectrometers. Chemical shifts for protons are reported in parts
per million (δ scale) and internally referenced to the CD3OD or CDCl3 signal at δ 3.33 and 7.28 ppm,
respectively. Mass spectral (MS) data were obtained using an Agilent
1100 LC/MSD VL system (G1946C) with a 0.4 mL/min flow rate using a
binary solvent system of 95:5 methyl alcohol/water. UV detection was
monitored at 254 nm. Mass spectra were acquired in positive and negative
mode scanning over the mass range. Elemental analyses (C, H, N) were
performed in house. Artemisinin, dihydroartemisinin, and artesunate
were obtained from Lachifarma s.r.l. (Zollino (LE), Italy).
in flame-dried glassware under a nitrogen atmosphere. Reagents were
obtained from commercial suppliers (Sigma-Aldrich Srl, Milan, Italy)
and used without further purification. TLC chromatography was performed
on precoated aluminum silica gel SIL G/UV254 plates (Macherey-Nagel
& Co.). The detection occurred via fluorescence quenching or development
in a molybdato phosphate solution (10% in EtOH). Merck silica gel
60 was used for flash chromatography (23–400 mesh). All products
were dried in high vacuum (10-3 mbar). 1H NMR and 13C NMR spectra were measured on a Bruker Avance
DRX400 (400 MHz/100 MHz) and on a Bruker Avance DPX200 (200 MHz/50
MHz) spectrometers. Chemical shifts for protons are reported in parts
per million (δ scale) and internally referenced to the CD3OD or CDCl3 signal at δ 3.33 and 7.28 ppm,
respectively. Mass spectral (MS) data were obtained using an Agilent
1100 LC/MSD VL system (G1946C) with a 0.4 mL/min flow rate using a
binary solvent system of 95:5 methyl alcohol/water. UV detection was
monitored at 254 nm. Mass spectra were acquired in positive and negative
mode scanning over the mass range. Elemental analyses (C, H, N) were
performed in house. Artemisinin, dihydroartemisinin, and artesunate
were obtained from Lachifarma s.r.l. (Zollino (LE), Italy).
6
Purification and Characterization of Organic Compounds
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All reactions were performed in flame-dried glassware under a nitrogen atmosphere. Reagents were obtained from commercial suppliers (Merck Srl, Milan, Italy) and used without further purification. TLC chromatography was performed on precoated aluminum silica gel SIL G/UV254 plates (Macherey-Nagel GmbH & Co. Düren, Germany). The detection occurred via fluorescence quenching or development in a ninhydrin solution (0.2 g of ninhydrin in 99.5 mL ethanol and 0.5 mL acetic acid.). Merck silica gel 60 was used for chromatography (23–400 mesh). 1H NMR and 13C NMR spectra were measured on a Bruker Avance DRX400 (400 MHz/100 MHz) spectrometer. Chemical shifts for protons were reported in parts per million (ppm, δ scale) and internally referenced to the deuterated dimethyl sulfoxide (DMSO-d6), methanol (CD3OD) or chloroform (CDCl3) signal at δ 2.50, 3.33 and 7.28 ppm, respectively. 1H-NMR spectra are reported in this order: multiplicity and number of protons. Signals were characterized as: s (singlet); d (doublet); dd (doublet of doublets); t (triplet); m (multiplet); bs (broad signal). Mass spectra were recorded with an Agilent 1100 LC/MSD VL system (G1946C) (Agilent Technologies, Palo Alto, CA, USA).
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