Electron spray ionization mass spectrometry and 2D 31P NMR for monitoring 18O/16O isotope exchange and turnover rates of metabolic oligophosphates

Emirhan Nemutlu, Nenad Juranic, Song Zhang, Lawrence E. Ward, Tumpa Dutta, K Sreekumaran Nair, Andre Terzic, Slobodan I Macura, Petras P Dzeja

Research output: Contribution to journalArticle

7 Citations (Scopus)

Abstract

A new method was here developed for the determination of 18O-labeling ratios in metabolic oligophosphates, such as ATP, at different phosphoryl moieties (α-, β-, and γ-ATP) using sensitive and rapid electrospray ionization mass spectrometry (ESI-MS). The ESI-MS-based method for monitoring of 18O/16O exchange was validated with gas chromatography-mass spectrometry and 2D 31P NMR correlation spectroscopy, the current standard methods in labeling studies. Significant correlation was found between isotopomer selective 2D 31P NMR spectroscopy and isotopomer less selective ESI-MS method. Results demonstrate that ESI-MS provides a robust analytical platform for simultaneous determination of levels, 18O-labeling kinetics and turnover rates of α-, β-, and γ-phosphoryls in ATP molecule. Such method is advantageous for large scale dynamic phosphometabolomic profiling of metabolic networks and acquiring information on the status of probed cellular energetic system.

Original languageEnglish (US)
Pages (from-to)697-706
Number of pages10
JournalAnalytical and Bioanalytical Chemistry
Volume403
Issue number3
DOIs
StatePublished - May 2012

Fingerprint

Electrospray ionization
Isotopes
Electrospray Ionization Mass Spectrometry
Ionization
Mass spectrometry
Mass Spectrometry
Nuclear magnetic resonance
Electrons
Monitoring
Labeling
Adenosine Triphosphate
Magnetic Resonance Spectroscopy
Metabolic Networks and Pathways
Gas chromatography
Gas Chromatography-Mass Spectrometry
Nuclear magnetic resonance spectroscopy
Spectroscopy
Molecules
Kinetics

Keywords

  • O isotope labeling
  • P NMR
  • ATP
  • Energy metabolism
  • ESI-MS
  • Phosphotransfer networks

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry

Cite this

Electron spray ionization mass spectrometry and 2D 31P NMR for monitoring 18O/16O isotope exchange and turnover rates of metabolic oligophosphates. / Nemutlu, Emirhan; Juranic, Nenad; Zhang, Song; Ward, Lawrence E.; Dutta, Tumpa; Nair, K Sreekumaran; Terzic, Andre; Macura, Slobodan I; Dzeja, Petras P.

In: Analytical and Bioanalytical Chemistry, Vol. 403, No. 3, 05.2012, p. 697-706.

Research output: Contribution to journalArticle

@article{ee1a3ac7f41a490ea93dd34630278e6c,
title = "Electron spray ionization mass spectrometry and 2D 31P NMR for monitoring 18O/16O isotope exchange and turnover rates of metabolic oligophosphates",
abstract = "A new method was here developed for the determination of 18O-labeling ratios in metabolic oligophosphates, such as ATP, at different phosphoryl moieties (α-, β-, and γ-ATP) using sensitive and rapid electrospray ionization mass spectrometry (ESI-MS). The ESI-MS-based method for monitoring of 18O/16O exchange was validated with gas chromatography-mass spectrometry and 2D 31P NMR correlation spectroscopy, the current standard methods in labeling studies. Significant correlation was found between isotopomer selective 2D 31P NMR spectroscopy and isotopomer less selective ESI-MS method. Results demonstrate that ESI-MS provides a robust analytical platform for simultaneous determination of levels, 18O-labeling kinetics and turnover rates of α-, β-, and γ-phosphoryls in ATP molecule. Such method is advantageous for large scale dynamic phosphometabolomic profiling of metabolic networks and acquiring information on the status of probed cellular energetic system.",
keywords = "O isotope labeling, P NMR, ATP, Energy metabolism, ESI-MS, Phosphotransfer networks",
author = "Emirhan Nemutlu and Nenad Juranic and Song Zhang and Ward, {Lawrence E.} and Tumpa Dutta and Nair, {K Sreekumaran} and Andre Terzic and Macura, {Slobodan I} and Dzeja, {Petras P}",
year = "2012",
month = "5",
doi = "10.1007/s00216-012-5899-5",
language = "English (US)",
volume = "403",
pages = "697--706",
journal = "Fresenius Zeitschrift fur Analytische Chemie",
issn = "0016-1152",
publisher = "Springer Verlag",
number = "3",

}

TY - JOUR

T1 - Electron spray ionization mass spectrometry and 2D 31P NMR for monitoring 18O/16O isotope exchange and turnover rates of metabolic oligophosphates

AU - Nemutlu, Emirhan

AU - Juranic, Nenad

AU - Zhang, Song

AU - Ward, Lawrence E.

AU - Dutta, Tumpa

AU - Nair, K Sreekumaran

AU - Terzic, Andre

AU - Macura, Slobodan I

AU - Dzeja, Petras P

PY - 2012/5

Y1 - 2012/5

N2 - A new method was here developed for the determination of 18O-labeling ratios in metabolic oligophosphates, such as ATP, at different phosphoryl moieties (α-, β-, and γ-ATP) using sensitive and rapid electrospray ionization mass spectrometry (ESI-MS). The ESI-MS-based method for monitoring of 18O/16O exchange was validated with gas chromatography-mass spectrometry and 2D 31P NMR correlation spectroscopy, the current standard methods in labeling studies. Significant correlation was found between isotopomer selective 2D 31P NMR spectroscopy and isotopomer less selective ESI-MS method. Results demonstrate that ESI-MS provides a robust analytical platform for simultaneous determination of levels, 18O-labeling kinetics and turnover rates of α-, β-, and γ-phosphoryls in ATP molecule. Such method is advantageous for large scale dynamic phosphometabolomic profiling of metabolic networks and acquiring information on the status of probed cellular energetic system.

AB - A new method was here developed for the determination of 18O-labeling ratios in metabolic oligophosphates, such as ATP, at different phosphoryl moieties (α-, β-, and γ-ATP) using sensitive and rapid electrospray ionization mass spectrometry (ESI-MS). The ESI-MS-based method for monitoring of 18O/16O exchange was validated with gas chromatography-mass spectrometry and 2D 31P NMR correlation spectroscopy, the current standard methods in labeling studies. Significant correlation was found between isotopomer selective 2D 31P NMR spectroscopy and isotopomer less selective ESI-MS method. Results demonstrate that ESI-MS provides a robust analytical platform for simultaneous determination of levels, 18O-labeling kinetics and turnover rates of α-, β-, and γ-phosphoryls in ATP molecule. Such method is advantageous for large scale dynamic phosphometabolomic profiling of metabolic networks and acquiring information on the status of probed cellular energetic system.

KW - O isotope labeling

KW - P NMR

KW - ATP

KW - Energy metabolism

KW - ESI-MS

KW - Phosphotransfer networks

UR - http://www.scopus.com/inward/record.url?scp=84862105178&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=84862105178&partnerID=8YFLogxK

U2 - 10.1007/s00216-012-5899-5

DO - 10.1007/s00216-012-5899-5

M3 - Article

VL - 403

SP - 697

EP - 706

JO - Fresenius Zeitschrift fur Analytische Chemie

JF - Fresenius Zeitschrift fur Analytische Chemie

SN - 0016-1152

IS - 3

ER -