Abstract
In this study, the hyphenation of LC-SPE-NMR-MS at 500 MHz was applied to the structural elucidation of a low concentrated paracetamol metabolite present in human urine. Single or multiple peak trapping of the mass detected metabolite on SPE cartridges was employed to increase the sensitivity and quality NMR measurement over the conventional LC-NMR method. After the elution of the metabolite from the SPE cartridge to the NMR flow probe using deuterated acetonitrile for initial NMR investigation, the fraction was revovered by flushing the sample out of the NMR probe head with nitrogen gas. On the recovered fraction, high resolution FT-ICR-MS measurements were conducted, giving exact mass information about the unknown metabolite. In addition, a cryogenic NMR micro probe head was used to enhance the sensitivity of the NMR measurement by a factor of 5 in order to run 2D experiments for structural elucidation of the unknown metabolite. The combination of both MS and NMR results, led unequivocally to the elucidation of the structure as the ether glucuronide of 3-methoxy-paracetamol.
Published Version
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a callDisclaimer: All third-party content on this website/platform is and will remain the property of their respective owners and is provided on "as is" basis without any warranties, express or implied. Use of third-party content does not indicate any affiliation, sponsorship with or endorsement by them. Any references to third-party content is to identify the corresponding services and shall be considered fair use under The CopyrightLaw.
