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Artifacts related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide derivatization of citrulline revealed by gas chromatography-mass spectrometry using both electron and chemical ionization.
J Chromatogr A. 2010 Aug 13; 1217(33):5444-8.JC

Abstract

Derivatization with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) was used for gas chromatography-mass spectrometry (GC-MS) analysis of citrulline and ornithine. Aqueous 50 microl aliquots at 1 and 10 mM concentrations were dried and derivatized separately, and 70 eV electron ionization or CH(4) positive chemical ionization were used. Ornithine produced a single GC peak. Physiological citrulline concentrations produced GC artifact peaks for the ornithine derivative, and a compound consistent with elimination of a water molecule from the tri-tert-butyldimethylsilyl (TBDMS) citrulline derivative. A third GC peak obtained using 10 mM citrulline concentrations gave a mass spectrum consistent with a mixture of true tri- and tetra-TBDMS citrulline. Analyses of (13)C-ureido-labeled citrulline confirmed the presence of the true TBDMS citrulline derivatives produced from 10 mM samples and provided evidence that the TBDMS ornithine artifact results from loss of TBDMS isocyanate from tetra-TBDMS citrulline. Linear-programmed temperature GC retention index data relative to n-alkanes are reported for observed GC peaks.

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Authors+Show Affiliations

Smith PA
Department of Preventive Medicine and Biometrics, Uniformed Services University of the Health Sciences, Bethesda, MD 20814-4712, USA. psmith@usuhs.mil
Villa V
No affiliation info available
King GL
No affiliation info available

MeSH

AcetamidesArginineArtifactsCitrullineFluoroacetatesGas Chromatography-Mass SpectrometryOrganosilicon CompoundsOrnithineTemperatureTrifluoroacetic Acid

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

20621299

Citation

Smith, Philip A., et al. "Artifacts Related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide Derivatization of Citrulline Revealed By Gas Chromatography-mass Spectrometry Using Both Electron and Chemical Ionization." Journal of Chromatography. A, vol. 1217, no. 33, 2010, pp. 5444-8.
Smith PA, Villa V, King GL. Artifacts related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide derivatization of citrulline revealed by gas chromatography-mass spectrometry using both electron and chemical ionization. J Chromatogr A. 2010;1217(33):5444-8.
Smith, P. A., Villa, V., & King, G. L. (2010). Artifacts related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide derivatization of citrulline revealed by gas chromatography-mass spectrometry using both electron and chemical ionization. Journal of Chromatography. A, 1217(33), 5444-8. https://doi.org/10.1016/j.chroma.2010.06.043
Smith PA, Villa V, King GL. Artifacts Related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide Derivatization of Citrulline Revealed By Gas Chromatography-mass Spectrometry Using Both Electron and Chemical Ionization. J Chromatogr A. 2010 Aug 13;1217(33):5444-8. PubMed PMID: 20621299.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Artifacts related to N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide derivatization of citrulline revealed by gas chromatography-mass spectrometry using both electron and chemical ionization. AU - Smith,Philip A, AU - Villa,Vilmar, AU - King,Gregory L, Y1 - 2010/06/23/ PY - 2010/04/26/received PY - 2010/06/15/revised PY - 2010/06/15/accepted PY - 2010/7/13/entrez PY - 2010/7/14/pubmed PY - 2010/10/29/medline SP - 5444 EP - 8 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1217 IS - 33 N2 - Derivatization with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA) was used for gas chromatography-mass spectrometry (GC-MS) analysis of citrulline and ornithine. Aqueous 50 microl aliquots at 1 and 10 mM concentrations were dried and derivatized separately, and 70 eV electron ionization or CH(4) positive chemical ionization were used. Ornithine produced a single GC peak. Physiological citrulline concentrations produced GC artifact peaks for the ornithine derivative, and a compound consistent with elimination of a water molecule from the tri-tert-butyldimethylsilyl (TBDMS) citrulline derivative. A third GC peak obtained using 10 mM citrulline concentrations gave a mass spectrum consistent with a mixture of true tri- and tetra-TBDMS citrulline. Analyses of (13)C-ureido-labeled citrulline confirmed the presence of the true TBDMS citrulline derivatives produced from 10 mM samples and provided evidence that the TBDMS ornithine artifact results from loss of TBDMS isocyanate from tetra-TBDMS citrulline. Linear-programmed temperature GC retention index data relative to n-alkanes are reported for observed GC peaks. SN - 1873-3778 UR - https://www.unboundmedicine.com/medline/citation/20621299/Artifacts_related_to_N_methyl_N__tert_butyldimethylsilyl_trifluoroacetamide_derivatization_of_citrulline_revealed_by_gas_chromatography_mass_spectrometry_using_both_electron_and_chemical_ionization_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(10)00830-7 DB - PRIME DP - Unbound Medicine ER -

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