MS Description
|
Extraction of metabolites<br />
The … Extraction of metabolites<br />
The freeze-dried samples were extracted with 50 μL of 80% MeOH containing 2.5 μM lidocaine per mg dry weight using a mixer mill (MM300, Retsch) with zirconia beads for 10 min at 20 Hz and 4 °C. After centrifugation for 10 min, the supernatant was filtered using an HLB μElution plate (Waters).<br />
<br />
LC–FTICR-MS Analysis<br />
A liquid sample (1 μL) was analyzed using LC–FTICR-MS (LC, Agilent 1200 series; MS, Bruker Daltonics solariX 7.0 T). Analytical conditions were as follows. LC: column, Xselect CSH C18 (3.5 μm, 2.1 mm ×150 mm, Waters); solvent system, solvent A (water with 0.1% formic acid) and solvent B (acetonitrile with 0.1% formic acid); gradient program, 99.5% A/0.5% B at 0 min, 0.5% A/99.5% B at 30.0 min, 0.5% A/99.5% B at 45.0 min, 99.5% A/0.5% B at 45.1 min, and 99.5% A/0.5% B at 60.0 min; flow rate, 0.3 mL/min; column temperature, 35 °C; wavelength, 200–600 nm; MS detection (resolution 260 000 at m/z 400, see Figure S1 in the Supporting Information); polarity, positive; calibrant, low concentration TuningMix (Agilent); lock mass target, diethylhexylphthalate (C24H38O4, [M + H]+m/z 391.28429); MS/MS detection (resolution 35 000 at m/z 400, see Figure S2 in the Supporting Information). Figure S2 in the Supporting Information).
|