Journal article
HPLC-SPE-NMR in pharmaceutical development: capabilities and applications
Magnetic resonance in chemistry, Vol.43(9), pp.762-770
09/2005
DOI: 10.1002/mrc.1615
PMID: 16049946
Abstract
High-performance liquid chromatography-solid phase extraction-NMR spectroscopy (HPLC-SPE-NMR) has recently become commercially available and has been evaluated with regard to its applicability in a pharmaceutical environment. The addition of an automated SPE unit to an HPLC-NMR system for peak trapping results in an improved NMR signal-to-noise ratio (S/N) and also has other practical advantages. The trapping efficiency is shown to depend on compound polarity and is highest for compounds eluting late on reversed-phase HPLC systems. Multiple peak trapping further increases the S/N, again with the best results for less polar compounds. For polar compounds, multiple peak trapping resulted in no S/N gain as the amount of material retained on the SPE cartridge was equivalent to that from a single injection. When compared with conventional HPLC-NMR, a S/N gain of up to five-fold could be achieved for some compounds in a single trapping step. A major advantage of the technique is the independence of the chromatographic step from the NMR step, resulting in greater versatility than conventional HPLC-NMR in the HPLC solvents and NMR solvents that can be used. Practical applications from both drug metabolite and drug impurity identification are presented.
Details
- Title: Subtitle
- HPLC-SPE-NMR in pharmaceutical development: capabilities and applications
- Creators
- Martin Sandvoss - DMPK Structural ID Group, GlaxoSmithKline R & D, Ware, UK. martin.x.sandvoss@gsk.comBen BardsleyTony L BeckEmma Lee-SmithStephanie E NorthPeter J Moore - GlaxoSmithKline (United Kingdom)Andrew J EdwardsRichard J Smith
- Resource Type
- Journal article
- Publication Details
- Magnetic resonance in chemistry, Vol.43(9), pp.762-770
- DOI
- 10.1002/mrc.1615
- PMID
- 16049946
- NLM abbreviation
- Magn Reson Chem
- ISSN
- 0749-1581
- eISSN
- 1097-458X
- Publisher
- England
- Language
- English
- Date published
- 09/2005
- Academic Unit
- Roy J. Carver Department of Biomedical Engineering; Molecular Physiology and Biophysics; Anatomy and Cell Biology; Stead Family Department of Pediatrics; Iowa Neuroscience Institute; Otolaryngology; Internal Medicine
- Record Identifier
- 9984007290602771
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