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. 2018 Aug 1;(138):57434. doi: 10.3791/57434
Liquid Chromatography
Column: reversed-phase C-18
Column: CoreShell column;
Column: 50 mm x 2.1 mm dimensions, 2.6 μm particle size
Column temperature 40 °C
Injection volume: 5 µL
Flow: 0.3 mL/min
Mobile phase: Solvent A: water containing 0.1% formic acid
Solvent B: methanol containing 0.1% formic acid
Gradient program:
Time /min 0 1 10 11.1 11.2 12
A:B solvent ratio 99:1 70:30 25:75 1:99 1:99 99:1
Mass Spectrometry
Source: Dual AJS ESI (positive mode)
Gas and source
Gas Temperature: 300 °C
Drying Gas: 8.0 L/min
Nebulizer: 14 psig
Sheath Gas Temperature: 300 °C
Sheath Gas Flow: 8 L/min
Mass Range: 100 - 1000 m/z
Acquisition Rate: 1 spectrum/s
Acquisition Time: 1000 ms/spectrum
Transient/ spectrum 10014
For targeted MS method
Collision energy (CE): 0 eV
Preferred Mass - Table 734.4685
For MS/MS (typically auto MS/MS mode)
Collision energy (CE): 30 eV
Absolute threshold 3000 counts
Relative threshold 0.01 %
Mass Range: 100 - 100 m/z
Acquisition Rate: 1 spectrum/s
Acquisition Time: 1000 ms/spectrum
Transient/ spectrum 9964
For targeted MS/MS method
Preferred Mass - Table 734.4685