Ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) equipped with a Waters Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7-μm particle size; Waters Corp., Millipore, Bedford, MA, United States) was used to detect the concentrations of flumatinib and M1. Quantification of the analytes was made by using a Waters XEVO TQS triple quadruple mass spectrometer with a multiple reaction monitoring (MRM) in positive ion mode. The mobile phase was consisted of 0.1% formic acid aqueous solution (A) and acetonitrile (B) at a flow rate of 0.4 mL/min. An elution program of 90% A (0–0.5 min), 90%–10% A (0.5–1.0 min), 10% A (1–1.5 min), 10%–90% A (1.5–1.6 min) and 90% A (1.6–2 min) was performed. The whole elution took 2 min. During the analysis, the temperature of the column and autosampler rack was controlled at 40°C and 10°C, respectively. In addition, optimized parameters for the mass spectra of flumatinib, M1 and dasatinib included: cone voltage were all 10 V, and collision energy was 20 eV, 25 eV, 20 eV, respectively. The monitoring transitions were m/z 563.1 → 463.0, m/z 549.3 → 462.9, and m/z 488.0 → 401.1 for flumatinib, M1 and dasatinib, respectively.
Xevo tq s triple quadruple mass spectrometer
Manufactured by Waters Corporation
The Xevo TQ-S is a triple quadrupole mass spectrometer designed for high-performance liquid chromatography (HPLC) and ultra-performance liquid chromatography (UPLC) applications. It features a high-sensitivity, high-resolution, and high-speed detection system for the accurate quantification and identification of a wide range of analytes.
Automatically generated - may contain errors
Lab products found in correlation
Targetlynx software, by Waters Corporation (2 mentions)
Acuity 1 class uplc system, by Waters Corporation (2 mentions)
8 μm uplc hss t3 column, by Waters Corporation (2 mentions)
1.8 μm uplc hss t3 pre column, by Waters Corporation (2 mentions)
Waters acquity uplc beh c18 column, by Waters Corporation (1 mentions)
Trifluoroacetic acid, by Merck Group (1 mentions)
4 protocols using xevo tq s triple quadruple mass spectrometer
1
Quantifying Flumatinib and Metabolite M1 by UPLC-MS/MS
2
LC-MS/MS Analysis of Nucleoside Monophosphates
3
LC-MS/MS Analysis of Nucleoside Monophosphates
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The LC-MS/MS instrument consisted of Acuity I-class UPLC system (Waters) and Xevo TQ-S triple quadruple mass spectrometer (Waters) equipped with an electrospray ion source and operated in positive ion mode was used for analysis of nucleoside monophosphates. MassLynx and TargetLynx software (v.4.1, Waters) were applied for the acquisition and analysis of data. Chromatographic separation was done on a 100 × 2.1-mm i.d., 1.8-μm UPLC HSS T3 column equipped with 50 × 2.1-mm i.d., 1.8-μm UPLC HSS T3 pre-column (both Waters Acuity) with mobile phases A (10 mM ammonium acetate and 5 mM ammonium hydrocarbonate buffer, pH 7.0 adjusted with 10% acetic acid) and B (acetonitrile) at a flow rate of 0.3 ml/min and column temperature 35°C. A gradient was as follows: 0–6 min the column was hold at 0% B, then 6-6.5 min linear increase till 100% B, 6.5-7.0 min hold at 100% B, 7.0-7.5 min back to 0% B and equilibration at 0% B for 2.5 minutes. Samples kept at 8°C were automatically injected in a volume of 3 μl.
For mass spectrometry argon was used as the collision gas with flow 0.25 ml/min. The capillary voltage was set to 2.90 kV, source temperature - 150°C, desolvation temperature - 350°C, desolvation gas flow - 650 L/min. Analytics were detected using multiple reaction monitoring (MRM) applying the parameters listed inSupplementary Table 1 .
For mass spectrometry argon was used as the collision gas with flow 0.25 ml/min. The capillary voltage was set to 2.90 kV, source temperature - 150°C, desolvation temperature - 350°C, desolvation gas flow - 650 L/min. Analytics were detected using multiple reaction monitoring (MRM) applying the parameters listed in
4
Quantification of Angiotensin Metabolites in Cardiac Tissue
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Angiotensin metabolites in cardiac tissue were quantified by Attoquant Diagnostics (Vienna, Austria) as described previously [13 (link)]. Frozen cardiac tissue segments (50–90 mg) were homogenized using pestle and mortar under liquid nitrogen. The frozen tissue powder was dissolved at 100 mg/ml in 6 mol/l aqueous guanidinium chloride supplemented with 1% (v/v) trifluoroacetic acid (Sigma-Aldrich) by cooled sonication using a 2 mm microtip (Sonics and Materials, Newton, NJ). Stable isotope-labeled internal standards for individual angiotensin metabolites (AngI, AngII) were added to tissue homogenates at 200 pg/ml. The samples then underwent C-18-based solid-phase extraction and were subjected to LC–MS/MS analysis using a reversed phase analytical column operating in line with a Xevo TQ-S triple quadruple mass spectrometer (Waters). Internal standards were used to correct for peptide recovery of the sample preparation procedure for each analyte in each individual sample. Analyte concentrations were reported in fmol/g and are calculated considering the corresponding response factors determined in appropriate calibration curves in original sample matrix, on condition that integrated signals exceeded a signal-to-noise ratio of 10.
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