MALDI MS was performed on an Ultraflex TOF-TOF (Bruker Daltonik) spectrometer as described previously (30 (link)). 2,5-Dihydroxybenzoic acid (Sigma–Aldrich) was used as a matrix. Measurements were performed in the reflectron mode with a mass accuracy error not exceeding 100 ppm. Mass spectra were analyzed with the Data Analysis 4.3 and Data Analysis Viewer 4.3 software (Bruker).
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MALDI-TOF Mass Spectrometry Protocol
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MALDI-TOF and ESI Mass Spectrometry
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Ultraflex TOF-TOF (Bruker Daltonik, Germany) spectrometer was used for MALDI mass spectrometry as described previously (Kuzmenkov et al., 2016b (link)). 2,5-Dihydroxybenzoic acid (Sigma-Aldrich) was used as a matrix. Measurements were performed in the linear mode. Mass spectra were analyzed with the Data Analysis 4.3 and Data Analysis Viewer 4.3 software (Bruker).
High-resolution mass spectra of activated p-HOBDI-BF2 were recorded on a TripleTOF 5600+ System (SCIEX) using electrospray ionization (ESI). The measurements were done in a positive ion mode (interface capillary voltage of 5500 V); mass range from m/z 50 to m/z 3,000; external or internal calibration was done with the ESI Tuning Mix (Agilent). A syringe injection was used for solutions in acetonitrile, methanol, or water (flow rate of 20 μl/min). Nitrogen was applied as a dry gas; interface temperature was set at 180°C.
ESI mass spectra of Aze fragments were recorded on an LTQ Orbitrap XL instrument (Thermo Fisher Scientific) equipped with HESI-II ion source. The acquisition was performed using full-scan FTMS mode at 30K resolution in a positive ions detection mode within the 700–2000 mass range.
High-resolution mass spectra of activated p-HOBDI-BF2 were recorded on a TripleTOF 5600+ System (SCIEX) using electrospray ionization (ESI). The measurements were done in a positive ion mode (interface capillary voltage of 5500 V); mass range from m/z 50 to m/z 3,000; external or internal calibration was done with the ESI Tuning Mix (Agilent). A syringe injection was used for solutions in acetonitrile, methanol, or water (flow rate of 20 μl/min). Nitrogen was applied as a dry gas; interface temperature was set at 180°C.
ESI mass spectra of Aze fragments were recorded on an LTQ Orbitrap XL instrument (Thermo Fisher Scientific) equipped with HESI-II ion source. The acquisition was performed using full-scan FTMS mode at 30K resolution in a positive ions detection mode within the 700–2000 mass range.
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