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

被引：24
作者：
Djukovic, Danijel [1 ]
Appiah-Amponsah, Emmanuel [1 ]
Shanaiah, Narasimhamurthy [1 ]
Gowda, G. A. Nagana [1 ]
Henry, Ian [1 ]
Everly, Mike [1 ]
Tobias, Brian [2 ]
Raftery, Daniel [1 ]
机构：
[1] Purdue Univ, Dept Chem, W Lafayette, IN 47907 USA
[2] Pfizer Inc, San Diego, CA 92121 USA
来源：
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS | 2008年 / 47卷 / 02期
关键词：
metabolite profiling; H-1; NMR; micro-coil; solid-phase extraction; ibuprofen;
D O I：
10.1016/j.jpba.2007.12.035
中图分类号：
O65 [分析化学];
学科分类号：
070302 ; 081704 ;
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. (c) 2008 Published by Elsevier B.V.
引用
收藏
页码：328 / 334
页数：7
相关论文
共 32 条
  • [1] Albert K., 2002, ON LINE LC NMR RELAT
  • [2] ONLINE COUPLING OF HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY AND NUCLEAR MAGNETIC-RESONANCE
    BAYER, E
    ALBERT, K
    NIEDER, M
    GROM, E
    [J]. JOURNAL OF CHROMATOGRAPHY, 1979, 186 (DEC): : 497 - 507
  • [3] HPLC/NMR in combinatorial chemistry
    Chin, J
    Fell, JB
    Jarosinski, M
    Shapiro, MJ
    Wareing, JR
    [J]. JOURNAL OF ORGANIC CHEMISTRY, 1998, 63 (02) : 386 - 390
  • [4] The application of high performance liquid chromatography, coupled to nuclear magnetic resonance spectroscopy and mass spectrometry (HPLC-NMR-MS), to the characterisation of ibuprofen metabolites from human urine
    Clayton, E
    Taylor, S
    Wright, B
    Wilson, ID
    [J]. CHROMATOGRAPHIA, 1998, 47 (5-6) : 264 - 270
  • [5] Combined HPLC-MS and HPLC-NMR on-line coupling for the separation and determination of lutein and zeaxanthin stereoisomers in spinach and in retina
    Dachtler, M
    Glaser, T
    Kohler, K
    Albert, K
    [J]. ANALYTICAL CHEMISTRY, 2001, 73 (03) : 667 - 674
  • [6] Application of directly coupled HPLC MMR to separation and characterization of lipoproteins from human serum
    Daykin, CA
    Corcoran, O
    Hansen, SH
    Bjornsdottir, I
    Cornett, C
    Connor, SC
    Lindon, JC
    Nicholson, JK
    [J]. ANALYTICAL CHEMISTRY, 2001, 73 (06) : 1084 - 1090
  • [7] Stereoselective determination of the major ibuprofen metabolites in human urine by off-line coupling solid-phase microextraction and high-performance liquid chromatography
    de Oliveira, ARM
    de Santana, FJM
    Bonato, PS
    [J]. ANALYTICA CHIMICA ACTA, 2005, 538 (1-2) : 25 - 34
  • [8] Signal enhancement in HPLC/microcoil NMR using automated column trapping
    Djukovic, Danijel
    Liu, Shuhui
    Henry, Ian
    Tobias, Brian
    Raftery, Daniel
    [J]. ANALYTICAL CHEMISTRY, 2006, 78 (20) : 7154 - 7160
  • [9] LC-NMR coupling technology: recent advancements and applications in natural products analysis
    Exarchou, V
    Krucker, M
    van Beek, TA
    Vervoort, J
    Gerothanassis, IP
    Albert, K
    [J]. MAGNETIC RESONANCE IN CHEMISTRY, 2005, 43 (09) : 681 - 687
  • [10] Characterization of a paracetamol metabolite using on-line LC-SPE-NMR-MS and a cryogenic NMR probe
    Godejohann, M
    Tseng, LH
    Braumann, U
    Fuchser, J
    Spraul, M
    [J]. JOURNAL OF CHROMATOGRAPHY A, 2004, 1058 (1-2) : 191 - 196
1234