SE57 > MS01
ID SE57_MS01
Title Acquisition of ESI-MS and ESI-MS/MS data, UPLC-TQMS analysis
Instrument Waters Xevo TQD, UPLC (Waters)
Instrument Type UPLC-QTOF-MS
Ionization Method ESI
Ion Mode N.A.
Description <Acquisition of ESI-MS and ESI-MS/MS data>

All the solutions of authentic compounds (250 μ M) were transferred from 10 ml vials to 1.2 ml glass inserts in 96-well plates (Webseal system, GL Sciences, Tokyo, Japan) and diluted to 50 pmol μ l –1 with H 2 O using an ALHS (Microlab STARplus, Hamilton, Reno, NV, USA). The solutions (20 μ l aliquots containing 1 nmol of compound) were analyzed by the flow injection method using a CTC-PAL injection system (AMR, Tokyo, Japan) and a Waters GI Pump solvent system (Waters, Milford, MA, USA) consisting of: 0.05 ml min –1 flow using a micro splitter (GL Sciences), 80% acetonitrile (0.1% formic acid) and 20% water (0.1% formic acid), with a 2.5 min cycle in the isocratic mode. The ionized authentic compounds were detected by TQMS (TQD, Waters) according to the following conditions: capillary voltage +3.0 keV or –2.8 keV, CV 10–60 eV (six levels), source temperature 120°C, desolvation temperature 350°C, cone gas fl ow 50 l h –1 , desolvation gas fl ow 600 l h –1 and CE 10–60 eV (six levels). A total of 61,920 spectra of 860 compounds were obtained.The optimal MRM conditions, including positive/negative polarity (e.g. [M] + , [M + H] + , [M] – , [M – H] – ), m / z of precursor ion and product ion, and optimal CV and CE were determined automatically for 497 of these compounds using the software QuanOptimize (Waters).

<UPLC-TQMS analysis>

The UPLC (Waters) conditions were manually optimized based on the separation patterns of 12 methionine-derived glucosinolates and were as follows: flow rate 0.24 ml min –1 ; solvents A, 0.1% formic acid in water and B, 0.1% formic acid in acetonitrile; gradient program of B (0 min, 0%; 0.25 min, 0%; 0.4 min, 9%; 0.8 min, 17%; 1.9 min, 100%; 2.1 min, 100%;
2.11 min, 0%); 3 min cycles with a temperature of 38°C.The TQMS detection conditions were the same as those for FIA-TQMS, except that the source temperature was 130°C.
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