High resolution mass spectrometry analysis of EASxOxO endoperoxides were performed in an UHPLC Agilent coupled to an UHR-ESI-Q-TOF Bruker Daltonics MaXis 3G mass spectrometer with CaptiveSpray source in the negative mode. The UHPLC mobile phase consisted of ammonium formate (solvent A) and acetonitrile:methanol 7:3, v/v (solvent B) with the following linear gradient: 25% B during 15 min, 25 to 70% B for 1 min, 70% B until 25 min, 70 to 25% B during 1 min and 25% B until 30 min. Endoperoxides was separated on a Luna C18 reverse phase column, 250 × 4.6 mm, 5 µM particle size (Phenomenex, Torance, CA) and monitored at 210 nm. The flow rate was 0.8 mL.min−1. Reverse phase column was kept at 30°C. The ESI conditions were: capillary, 4.0 kV; dry heater, 180 °C; dry gas, 8.0 l/min; end plate, −450 V. Nitrogen was used as collision gas and the CID (collision-induced dissociation) energy was 10 eV. The instrument was externally calibrated using an ESI low concentration tuning mix over the m/z range of 100 to 2000. The Bruker Data Analysis software (version 4.0) was employed for data acquisition and processing.
Maxis 3g mass spectrometer
Manufactured by Bruker
Sourced in United States
The MaXis 3G mass spectrometer is a high-resolution quadrupole time-of-flight (Q-TOF) mass spectrometer designed for accurate mass measurements and comprehensive structural analysis of a wide range of analytes. The instrument features an innovative ion optic design, high-speed data acquisition, and advanced software for data processing and interpretation.
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2 protocols using maxis 3g mass spectrometer
1
UHPLC-HRMS Analysis of EAS^xO^xO Endoperoxides
2
Mass Spectrometry and NMR Analysis of Biomolecules
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Mass spectrometry analysis was performed on a Shimadzu model CBM-20A chromatograph, equipped with Shimadzu LC-20AD pumps, a Shimadzu SPD-20A detector, Shimadzu CTO-20A oven, Shimadzu SIL 20AC autoinjector, and Bruker Daltonics maXis 3G mass spectrometer (Bruker Corp., Billerica, MA, USA), with a 4500-V capillary, 2-bar nebulizers, at 200°C, and a gas flow of 8 liter/min−1 operating in MS and MS/MS data acquisition mode with the electron spray source in positive mode (ESI+). For the liquid chromatography, a reverse-phase C18 (Phenomenex Luna) plus column (250 mm × 4.6 mm × 5 μm) was used, with a flow rate of 1.0 ml.min−1. The elution system used a gradient system which consisted of a mixture of (i) acidified water (TFA 0.05%) and (ii) acetonitrile (ACN) for 10 to 70 min, reaching 80% ACN (48 ).
Nuclear magnetic resonance (NMR) was performed using a Bruker III 500-MHz spectrometer in deuterated water (D2O), and the results were analyzed by unidimensional (1D) 1H NMR and two-dimensional (2D) heteronuclear single quantum coherence (HSQC) and heteronuclear multiple-bond correlation (HMBC) (48 ).
Nuclear magnetic resonance (NMR) was performed using a Bruker III 500-MHz spectrometer in deuterated water (D2O), and the results were analyzed by unidimensional (1D) 1H NMR and two-dimensional (2D) heteronuclear single quantum coherence (HSQC) and heteronuclear multiple-bond correlation (HMBC) (48 ).
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