HPLC-SPE-NMR in pharmaceutical development: capabilities and applications
| Autor: | Richard J. Smith, Ben Bardsley, Tony L. Beck, Stephanie E. North, Emma Lee-Smith, Martin Sandvoss, Peter J. Moore, Andrew J. Edwards |
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| Rok vydání: | 2005 |
| Předmět: |
Chromatography
Acetonitriles Magnetic Resonance Spectroscopy Chemistry Chemical polarity Analytical chemistry Acids Carbocyclic General Chemistry Trapping Ketones High-performance liquid chromatography Sensitivity and Specificity Rats Cartridge Dogs Pharmaceutical Preparations Phase (matter) Drug Impurity Solvents Animals Bile General Materials Science Solid phase extraction Spectroscopy Chromatography High Pressure Liquid |
| Zdroj: | Magnetic resonance in chemistry : MRC. 43(9) |
| ISSN: | 0749-1581 |
| Popis: | 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. |
| Databáze: | OpenAIRE |
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