Agilent 1260 6460 triple quadrupole lc ms system

HPLC analyses were carried out with an Apollo C18 column (5 μm, 4.6
× 250mm, Alltech, Deerfield, IL, USA) with Shimadzu HPLC system
(Shimadzu, Kyoto, Japan). The column was developed with a linear gradient using
acetonitrile and water with 0.1% trifluoroacetic acid at a flow rate of 0.8
mL/min. For the first 5 minutes, the ratio of acetonitrile was maintained at 5%,
and it was changed linearly from 5% to 90% over 5–25 min and from 90% to
100% over 25–30 min. The detection wavelength was 320 nm.
MS and tandem MS were performed on an Agilent 1260/6460 Triple-Quadrupole LC/MS
system (Agilent, Santa Clara, CA, USA) with the electrospray ionization source.
The high resolution MS analysis was performed on an Aligent 1200 HPLC system and
6520 QTF-MS system (Agilent, Santa Clara, CA, USA). The mass spectrometer
scanned from m/z = 100–1500 in negative ion mode.

HPLC analyses were carried out with an Apollo C18 column (5 μm, 4.6 mm × 250 mm, Alltech, Deerfield, IL, USA) on a Shimadzu HPLC system (Shimadzu, Kyoto, Japan). Briefly, the column was developed with solution A (water with 0.1% trifluoroacetic acid) and acetonitrile at a flow rate of 0.8 mL/min. The percentage of acetonitrile was changed using the following gradient: 0–5 min, 10%; 5–25 min, 10%–90%; 25–30 min, 90%–100%; 30–35 min, 100%. The detection wavelength was 320 nm. LC-MS analyses were performed on an Agilent 1260/6460 Triple-Quadrupole LC/MS system (Santa Clara, CA, USA) with an electrospray ionization source. HR-ESI-MS was performed on an Agilent 1260 HPLC/6520 QTOF-MS instrument (Santa Clara, CA, USA). NMR spectra were recorded at room temperature on a Bruker-500 NMR spectrometer (Billerica, MA, USA).

HPLC detection of AFN congeners was performed on a Shimadzu HPLC system (Shimadzu, Kyoto, Japan) by an Apollo C₁₈ column (5 μm, 4.6 mm × 250 mm, Alltech, Deerfield, IL, United States). The Apollo C₁₈ column was eluted with acetonitrile and water containing 0.1% trifluoroacetic acid at a flow rate of 1.0 mL/min. Percentage of acetonitrile was changed linearly from 15 to 50% in 5 min, from 50 to 87% in 25 min, 87% for 5 min, and from 87 to 100% in 5 min. The detection wavelength was 220 nm. LC-MS analyses were performed on an Agilent 1260/6460 Triple-Quadrupole LC/MS system (Santa Clara, CA, United States) with an electrospray ionization source. HR-ESI-MS was performed on an Agilent 1260 HPLC/6520 QTOF-MS instrument (Santa Clara, CA, United States). NMR spectra were recorded at room temperature on a Bruker-500 NMR spectrometer (Billerica, MA, United States).