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Sample Set Information

Title LC-MS analysis of 15 vegetables and fruits
Description This study is aimed to a comprehensive annotation of metabolites in major vegetables and fruits produced in Japan.
Authors Sakurai N 1, Suda K 1, and Takahashi S 2 (1 Kazusa DNA Research Institute, 2 KAGOME CO. LTD.)
Reference Akimoto N, Ara T, Nakajima D, Suda K, Ikeda C, Takahashi S, Muneto R, Yamada M, Suzuki H, Shibata D, Sakurai N (2017) FlavonoidSearch: A system for comprehensive flavonoid annotation by mass spectrometry. Scientific Reports 7: 1243

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Sample Information

ID S99
Title Mock
Organism - Scientific Name
Organism - ID
Compound - ID
Compound - Source
Sample Preparation Details ID
Comment The same procedure of metabolite extraction and analysis were performed without plant materials.

Analytical Method Information

Title Mock1
Method Details ID MS1
Sample Amount 20 ul injected
Comment An independent preparation of the mock sample was performed for this instrumental analysis.

[MassBase ID] MDLC1_47241

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The raw (binary) and near-raw (text) files of this analysis are available at MassBase.

Analytical Method Details Information

Title LC-FT-MS, ESI, Positive (method 1)
Instrument Agilent1100 HPLC (Agilent), LTQ-FT (Thermo Fisher Scientific)
Instrument Type LC-FTICR-MS
Ionization ESI
Ion Mode Positive
Description Freeze-dried powder of plant material was extracted with 75% methanol containing 25 µM of 7-hydroxy-5-methylflavone as an internal standard. After homogenization using a Mixer Mill MM 300 (Quiagen) at 25 Hz for 2 min twice, homogenates were centrifuged (17,400 g, 5 min, 4 ºC). The supernatant was filtered through 0.2 µm PTFE membrane (Millipore). Hydrophobic compounds in the filtrate were removed by absorbing to C18 silica column (MonoSpin C18, GL Science, Tokyo, Japan).

Mock sample was prepared with the same procedure without adding the plant material and with 100% methanol containing 25 µM of 7-hydroxy-5-methylflavone as an internal standard.

20 µl of methanol solution was applied to a TSK-gel column ODS-100V (4.6 x 250 mm, 5 µm; TOSOH). Water (HPLC grade; solvent A) and acetonitrile (HPLC grade; solvent B) were used as the mobile phase with 0.1% v/v formic acid added to both solvents. The gradient program was as follows: 3% B (0 min), 97% B (90 min), 97% B (100 min), 3% B (100.1), and 3% B (107 min). The flow rate was set to 0.25 ml/min (0-100 min) and 0.5 ml/min (100.1-107 min). The flow rate was set to 0.5 ml/min, and the column oven temperature was set at 40 ºC. Compounds are detected in ESI-positive mode in the range m/z 100-1500. Multistage MSn analyses were carried out using collision induced dissociation (CID) in a linear ion trap detector at a normalized collision energy of 35.0% and an isolation width of 4.0 (m/z), and monitored by both ion trap detector and FT-ICR detector at 25,000 (at m/z 400) mass resolution. The ESI setting was as follows: spray voltage 4.0 kV and capillary temperature 300 ºC. Nitrogen sheath gas and auxiliary gas were set at 40 and 15 arbitrary units, respectively. To monitor HPLC elution, a photodiode array detector was used in the wavelength range 200–650 nm.

Mass scan events were set as follows (referred as method 1): full mass scan with FT-ICR in resolution 100,000 and MS2 scans for the most intense 5 ions of full mass scan with ion trap (IT). A dynamic exclusion setting was applied as follows: repeat count, 3; repeat duration, 30 sec; exclusion list size, 500; margin, 10 ppm, and exclusion duration, 20.

The data were acquired by Xcalibur software version 2.07 (Thermo Fisher Scientific).

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