SPE-NMR metabolite sub-profiling of urine

D.M. Jacobs, L. Spiesser, M. Garnier, N. de Roo, F. van Dorsten, B. Hollebrands, E. van Velzen, R. Draijer, J.P.M. van Duynhoven

Research output: Contribution to journalArticleAcademicpeer-review

23 Citations (Scopus)

Abstract

NMR-based metabolite profiling of urine is a fast and reproducible method for detection of numerous metabolites with diverse chemical properties. However, signal overlap in the (1)H NMR profiles of human urine may hamper quantification and identification of metabolites. Therefore, a new method has been developed using automated solid-phase extraction (SPE) combined with NMR metabolite profiling. SPE-NMR of urine resulted in three fractions with complementary and reproducible sub-profiles. The sub-profile from the wash fraction (100 % water) contained polar metabolites; that from the first eluted fraction (10 % methanol-90 % water) semi-polar metabolites; and that from the second eluted fraction (100 % methanol) aromatic metabolites. The method was validated by analysis of urine samples collected from a crossover human nutritional intervention trial in which healthy volunteers consumed capsules containing a polyphenol-rich mixture of red wine and grape juice extract (WGM), the same polyphenol mixture dissolved in a soy drink (WGM_Soy), or a placebo (PLA), over a period of five days. Consumption of WGM clearly increased urinary excretion of 4-hydroxyhippuric acid, hippuric acid, 3-hydroxyphenylacetic acid, homovanillic acid, and 3-(3-hydroxyphenyl)-3-hydroxypropionic acid. However, there was no difference between the excreted amounts of these metabolites after consumption of WGM or WGM_Soy, indicating that the soy drink is a suitable carrier for WGM polyphenols. Interestingly, WGM_Soy induced a significant increase in excretion of cis-aconitate compared with WGM and PLA, suggesting a higher demand on the tricarboxylic acid cycle. In conclusion, SPE-NMR metabolite sub-profiling is a reliable and improved method for quantification and identification of metabolites in urine to discover dietary effects and markers of phytochemical exposure
Original languageEnglish
Pages (from-to)2349-2361
Number of pages13
JournalAnalytical and Bioanalytical Chemistry
Volume404
Issue number8
DOIs
Publication statusPublished - 2012

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Solid Phase Extraction
Metabolites
Nuclear magnetic resonance
Urine
Polyphenols
Methanol
Aconitic Acid
Placebos
Homovanillic Acid
Citric Acid Cycle
Water
Vitis
Phytochemicals
Wine
Capsules
Healthy Volunteers
Chemical properties

Keywords

  • red wine
  • nutrition research
  • metabolomics
  • polyphenols
  • gut
  • humans
  • health
  • impact
  • milk
  • identification

Cite this

Jacobs, D. M., Spiesser, L., Garnier, M., de Roo, N., van Dorsten, F., Hollebrands, B., ... van Duynhoven, J. P. M. (2012). SPE-NMR metabolite sub-profiling of urine. Analytical and Bioanalytical Chemistry, 404(8), 2349-2361. https://doi.org/10.1007/s00216-012-6339-2
Jacobs, D.M. ; Spiesser, L. ; Garnier, M. ; de Roo, N. ; van Dorsten, F. ; Hollebrands, B. ; van Velzen, E. ; Draijer, R. ; van Duynhoven, J.P.M. / SPE-NMR metabolite sub-profiling of urine. In: Analytical and Bioanalytical Chemistry. 2012 ; Vol. 404, No. 8. pp. 2349-2361.
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Jacobs, DM, Spiesser, L, Garnier, M, de Roo, N, van Dorsten, F, Hollebrands, B, van Velzen, E, Draijer, R & van Duynhoven, JPM 2012, 'SPE-NMR metabolite sub-profiling of urine', Analytical and Bioanalytical Chemistry, vol. 404, no. 8, pp. 2349-2361. https://doi.org/10.1007/s00216-012-6339-2

SPE-NMR metabolite sub-profiling of urine. / Jacobs, D.M.; Spiesser, L.; Garnier, M.; de Roo, N.; van Dorsten, F.; Hollebrands, B.; van Velzen, E.; Draijer, R.; van Duynhoven, J.P.M.

In: Analytical and Bioanalytical Chemistry, Vol. 404, No. 8, 2012, p. 2349-2361.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - SPE-NMR metabolite sub-profiling of urine

AU - Jacobs, D.M.

AU - Spiesser, L.

AU - Garnier, M.

AU - de Roo, N.

AU - van Dorsten, F.

AU - Hollebrands, B.

AU - van Velzen, E.

AU - Draijer, R.

AU - van Duynhoven, J.P.M.

PY - 2012

Y1 - 2012

N2 - NMR-based metabolite profiling of urine is a fast and reproducible method for detection of numerous metabolites with diverse chemical properties. However, signal overlap in the (1)H NMR profiles of human urine may hamper quantification and identification of metabolites. Therefore, a new method has been developed using automated solid-phase extraction (SPE) combined with NMR metabolite profiling. SPE-NMR of urine resulted in three fractions with complementary and reproducible sub-profiles. The sub-profile from the wash fraction (100 % water) contained polar metabolites; that from the first eluted fraction (10 % methanol-90 % water) semi-polar metabolites; and that from the second eluted fraction (100 % methanol) aromatic metabolites. The method was validated by analysis of urine samples collected from a crossover human nutritional intervention trial in which healthy volunteers consumed capsules containing a polyphenol-rich mixture of red wine and grape juice extract (WGM), the same polyphenol mixture dissolved in a soy drink (WGM_Soy), or a placebo (PLA), over a period of five days. Consumption of WGM clearly increased urinary excretion of 4-hydroxyhippuric acid, hippuric acid, 3-hydroxyphenylacetic acid, homovanillic acid, and 3-(3-hydroxyphenyl)-3-hydroxypropionic acid. However, there was no difference between the excreted amounts of these metabolites after consumption of WGM or WGM_Soy, indicating that the soy drink is a suitable carrier for WGM polyphenols. Interestingly, WGM_Soy induced a significant increase in excretion of cis-aconitate compared with WGM and PLA, suggesting a higher demand on the tricarboxylic acid cycle. In conclusion, SPE-NMR metabolite sub-profiling is a reliable and improved method for quantification and identification of metabolites in urine to discover dietary effects and markers of phytochemical exposure

AB - NMR-based metabolite profiling of urine is a fast and reproducible method for detection of numerous metabolites with diverse chemical properties. However, signal overlap in the (1)H NMR profiles of human urine may hamper quantification and identification of metabolites. Therefore, a new method has been developed using automated solid-phase extraction (SPE) combined with NMR metabolite profiling. SPE-NMR of urine resulted in three fractions with complementary and reproducible sub-profiles. The sub-profile from the wash fraction (100 % water) contained polar metabolites; that from the first eluted fraction (10 % methanol-90 % water) semi-polar metabolites; and that from the second eluted fraction (100 % methanol) aromatic metabolites. The method was validated by analysis of urine samples collected from a crossover human nutritional intervention trial in which healthy volunteers consumed capsules containing a polyphenol-rich mixture of red wine and grape juice extract (WGM), the same polyphenol mixture dissolved in a soy drink (WGM_Soy), or a placebo (PLA), over a period of five days. Consumption of WGM clearly increased urinary excretion of 4-hydroxyhippuric acid, hippuric acid, 3-hydroxyphenylacetic acid, homovanillic acid, and 3-(3-hydroxyphenyl)-3-hydroxypropionic acid. However, there was no difference between the excreted amounts of these metabolites after consumption of WGM or WGM_Soy, indicating that the soy drink is a suitable carrier for WGM polyphenols. Interestingly, WGM_Soy induced a significant increase in excretion of cis-aconitate compared with WGM and PLA, suggesting a higher demand on the tricarboxylic acid cycle. In conclusion, SPE-NMR metabolite sub-profiling is a reliable and improved method for quantification and identification of metabolites in urine to discover dietary effects and markers of phytochemical exposure

KW - red wine

KW - nutrition research

KW - metabolomics

KW - polyphenols

KW - gut

KW - humans

KW - health

KW - impact

KW - milk

KW - identification

U2 - 10.1007/s00216-012-6339-2

DO - 10.1007/s00216-012-6339-2

M3 - Article

VL - 404

SP - 2349

EP - 2361

JO - Analytical and Bioanalytical Chemistry

JF - Analytical and Bioanalytical Chemistry

SN - 1618-2642

IS - 8

ER -

Jacobs DM, Spiesser L, Garnier M, de Roo N, van Dorsten F, Hollebrands B et al. SPE-NMR metabolite sub-profiling of urine. Analytical and Bioanalytical Chemistry. 2012;404(8):2349-2361. https://doi.org/10.1007/s00216-012-6339-2