Ibuprofen metabolite profiling using a combination of SPE/column-trapping and HPLC–micro-coil NMR

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• 作者：Danijel Djukovic ; Emmanuel Appiah-Amponsah ; Narasimhamurthy Shanaiah ; G.A. Nagana Gowda ; Ian Henry ; Mike Everly ; Brian Tobias ; Daniel Raftery
• 关键词：Metabolite profiling ; ¹H NMR ; Micro-coil ; Solid-phase extraction ; Ibuprofen
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2008
• 期刊代码：65_07317085
• 类别：ch
• 出版时间：9 June 2008
• 卷：47
• 期：2
• 页码：328-334
• 文件大小：542 K

摘要

Solid-phase extraction and column-trapping preconcentration are combined to enhance HPLC–nuclear magnetic resonance (HPLC–NMR) and applied to metabolite profiling in biological samples. Combining the two signal enhancement techniques improved the NMR signal substantially such that we were able to identify 2-hydroxyibuprofen, carboxyibuprofen, and unmetabolized ibuprofen molecules from a small urine sample after a therapeutic dose of ibuprofen. The hyphenated SPE/column-trapping method resulted in an excellent overall signal enhancement of up to 90-fold.