Potential of CE/MS for Small Carboxylic Acids Analysis as Alternative to GC/MS Reference Analytical MethodsFar, Johann ; ; et alPoster (2012, October) GC/MS (Gas Chromatography coupled to Mass Spectrometry) is the analytical method of choice for carboxylic acids analysis because of good sensitivity, low limit of detection and the possibility to compare ... [more ▼] GC/MS (Gas Chromatography coupled to Mass Spectrometry) is the analytical method of choice for carboxylic acids analysis because of good sensitivity, low limit of detection and the possibility to compare the pattern of fragmentation with existing databases for identification. However GC requires that the analytes are volatile. If it is not the case, the use of chemicals in order to perform the derivatization is mandatory, this may induce analytical bias. CE (Capillary electrophoresis) is a technique of choice for ions separation without prior treatments. The method is fast and do not require highly technical skills. A UV detector is the most common detection method; however electrospray mass spectrometry detection is recently gaining interest, while it really helps for structural information of the detected compounds. In this poster, the preliminary results of CE/MS analysis of several carboxylic acids are presented. All carboxylic acids are analyzed without any sample pretreatment. These acids looked at are from the “Citric Acid Cycle” including pyruvate and some isotope labeled analogues but also glyoxylate, lactate, oxalate and tartrate. Moreover, the preliminary results of a sample preparation approach to remove phosphate salts are presented. Phosphate is a very common salt that is often used in biological buffers but prevents the derivatization of carboxylic acid for GC/MS analysis and reduces the reproducibility of results for both GC/MS and CE/MS analysis. [less ▲] Detailed reference viewed: 14 (1 ULg) Large-scale identification of selenium metabolites by online size-exclusion-reversed phase liquid chromatography with combined inductively coupled plasma (ICP-MS) and electrospray ionization linear trap-Orbitrap mass spectrometry (ESI-MS(n)); Far, Johann ; et alin Metallomics (2012), 4(5), 422-432 A method was developed for the comprehensive cartography of the selenium metabolites synthesized in the process of conversion of selenite [Se(IV)] into organic compounds and enrichment of yeast with ... [more ▼] A method was developed for the comprehensive cartography of the selenium metabolites synthesized in the process of conversion of selenite [Se(IV)] into organic compounds and enrichment of yeast with selenium. The number of compounds detected was considerably increased (49) owing to the optimization of the fractionation procedure and the use of UPLC. The increased purity of the minor selenoorganic amino acids and oligopeptides allowed successful on-line de-novo identification based on the exact mass (o1 ppm) and fragmentation (MS2/MS3) mass spectra obtained with high resolution and high mass accuracy. The quality of mass spectra allowed the re-interpretation of previously reported structures of some selenium species. [less ▲] Detailed reference viewed: 10 (1 ULg) The usefulness of Ion Mobility-Mass Spectrometry for Small Molecules AnalysisFar, Johann ; Goscinny, Séverine ; et alConference (2012, March) Detailed reference viewed: 34 (6 ULg) Recent advances in analytical chemistry and mass spectrometry for organic selenium and tellurium compoundsFar, Johann ; De Pauw, Edwin ; Eppe, Gauthier ![]() in Rappoport, Zvi (Ed.) The Chemistry of Organic Selenium and Tellurium compounds Volume 3 Part 1 and 2 (2012) The objective of this chapter is to present the recent developments in mass spectrometry for selenium (Se) and tellurium (Te) analysis. The state-of-the-art of mass spectrometry based techniques available ... [more ▼] The objective of this chapter is to present the recent developments in mass spectrometry for selenium (Se) and tellurium (Te) analysis. The state-of-the-art of mass spectrometry based techniques available is critically evaluated with particular emphasis in ion sources and mass analyzers. The complexity of identification and characterization of Se, Te species including their speciation in the environment or in biological materials requires methodologies not only limited to mass spectrometry. Particular attention is given to sample preparation and hyphenated techniques with mass spectrometry for a comprehensive characterization of these trace elements. All these aspects are illustrated with up-to-date applications from the literature. Finally, future trends in mass spectrometry give the readers new insights in Se and Te species detection. [less ▲] Detailed reference viewed: 37 (3 ULg) Characterization of isomers selenium containing compounds and determination of isomer ratio from Se-rich yeast water extract using electrospray ionization and Ion Mobility Mass SpectrometryFar, Johann ; De Pauw, Edwin ; et alConference (2011, June) Detailed reference viewed: 10 (0 ULg) Contribution of multidimensional liquid chromatography with Inductively Coupled Plasma Mass Spectrometry and Ion Mobility Mass Spectrometry detection in speciation analyses of selenium containing from selenium-rich yeastsFar, Johann ; ; De Pauw, Edwin et alPoster (2011, June) Detailed reference viewed: 8 (0 ULg) Structural characterization of isobar selenium containing contaminant in a commercially available selenomethionine standard using electrospray – Ion Mobility Time of Flight Mass SpectrometryFar, Johann ; Mazzucchelli, Gabriel ; De Pauw, Edwin et alPoster (2011, April) Detailed reference viewed: 12 (0 ULg) Mass spectrometry applied to biomolecules analysisFar, Johann ; Mazzucchelli, Gabriel ; Meuwis, Marie-Alice et alConference (2011, March 31) Detailed reference viewed: 5 (3 ULg) Characterization of a selenium containing contaminant in a commercially available selenomethionine standard by ElectroSpray Ionization Ion Mobility Mass SpectrometryFar, Johann ; Mazzucchelli, Gabriel ; De Pauw, Edwin et alConference (2011) Detailed reference viewed: 10 (1 ULg) Study of the Se-containing metabolomes in Se-rich yeast by size-exclusion-cation-exchange HPLC with the parallel ICP MS and electrospray orbital ion trap detection; Far, Johann ; et alin Metallomics (2010), 2(8), 535-548 Strong cation exchange HPLC with the parallel ICP MS and electrospray hybrid linear ion trap quadrupole orbital trap mass spectrometry (ESI Orbitrap MS) detection was developed for the study of the ... [more ▼] Strong cation exchange HPLC with the parallel ICP MS and electrospray hybrid linear ion trap quadrupole orbital trap mass spectrometry (ESI Orbitrap MS) detection was developed for the study of the metabolomic pattern of selenium in selenium-rich yeast. The mobile phase composition (gradient of ammonium formate in 20% methanol) was optimized to obtain separation in conditions guaranteeing the identical ICP MS sensitivity during the entire chromatographic run and the compatibility with electrospray ionization. Twenty seven Se-containing metabolites observed in the HPLC-ICP MS chromatogram were identified by ESI Orbitrap MS based on the Se isotopic pattern, the accurate molecular mass, and the multistage fragmentation patterns. The method allowed for the first time the correlation of the differences observed in HPLC-ICP MS chromatography of water extracts of Se-rich yeast samples from different manufacturers with the identity of the eluted compounds determined by ESI MS. [less ▲] Detailed reference viewed: 15 (3 ULg) Determination of the selenium isotopic compositions in Se-rich yeast by hydride generation-inductively coupled plasma multicollector mass spectrometryFar, Johann ; ; et alin Journal of Analytical Atomic Spectrometry [=JAAS] (2010), 25(11), 1695-1703 A method was developed for the precise determination of selenium isotopic compositions (delta Se-82/77, delta Se-82/76 and delta Se-82/74) by hydride generation inductively coupled plasma multiple ... [more ▼] A method was developed for the precise determination of selenium isotopic compositions (delta Se-82/77, delta Se-82/76 and delta Se-82/74) by hydride generation inductively coupled plasma multiple collector mass spectrometry (HG-MC ICP MS) in Se-rich yeast. The conversion of all the selenium forms into Se(IV) during digestion and reduction steps was investigated by anion-exchange ICP quadrupole MS (SAX ICP Q MS) and was found to be complete. Measurement precision values expressed as deltas (delta) with regard to NIST SR M3149 were between 0.2-0.4 parts per thousand (2SD) over a period of 6 months for 25 or 50 ng mL(-1) of introduced selenium. The application of the method to the analysis of nine Se-rich yeast supplements from different manufactures showed significant variations in the isotope ratios suggesting that the latter can be an attractive parameter for the yeast provenance discrimination. [less ▲] Detailed reference viewed: 8 (3 ULg) Detection and identification of hydrophilic selenium compounds in selenium-rich yeast by size exclusion-microbore normal-phase HPLC with the on-line ICP-MS and electrospray Q-TOF-MS detectionFar, Johann ; ; in Analytica Chimica Acta (2010), 657(2), Normal-phase HPLC and hydrophilic interaction HPLC (HILIC) were investigated for the separation of selenometabolites in a water extract of Se-rich yeast prior to their detection by ICP-MS and ... [more ▼] Normal-phase HPLC and hydrophilic interaction HPLC (HILIC) were investigated for the separation of selenometabolites in a water extract of Se-rich yeast prior to their detection by ICP-MS and identification by electrospray MS/MS. The targeted fraction was a low-abundant fraction co-eluting with salt and sulfur analogues in size-exclusion chromatography which has so far been inaccessible to Se speciation studies. The optimization of the separation conditions resulted in the highest separation efficiency when HILIC was used and elution was carried out isocratically with a low concentration ammonium acetate buffer (1 mM ammonium acetate/10mM acetic acid) in 80% acetonitrile. Out of 15 peaks observed with the Se-specific ICP-MS detection 12 was identified by electrospray Q-TOF MS/MS (2,3-dihydroxypropionyl (DHP)-Se-methylselenocysteine [M+H](+): 272, Se-methyl-gamma-glutamyl-selenocysteinylglycine dioxide [M+H](+): 402, gamma-glutanlyl-Se-methylselenocysteine[M+H](+): 313; isomers of gamma-glutamylselenocystathionine [M+H](+): 400; Se-methyl-selenoglutathione [M+H](+): 370, isomers of N-acetylselenocystathionine [M+H](+): 313, 2,3-DHP-selenohomolanthionine [M+H](+): 373, isomers of 2,3-DHP-seienocystathionine[M+H](+): 359,2,3-DHP-selenolanthionine [M+H](+): 345 and selenohomolanthionine [M+H](+): 285). (C) 2009 Elsevier B.V. All rights reserved. [less ▲] Detailed reference viewed: 17 (4 ULg) Identification of anionic selenium species in Se-rich yeast by electrospray QTOF MS/MS and hybrid linear ion trap/orbitrap MSn; Far, Johann ; in Metallomics (2009), 1(4), 317-329 An analytical approach allowing the identification Of unknown selenium metabolites ill selenium-rich yeast was described. Anion-exchange HPLC of the Se-metabolome fraction co-eluting with salts ill size ... [more ▼] An analytical approach allowing the identification Of unknown selenium metabolites ill selenium-rich yeast was described. Anion-exchange HPLC of the Se-metabolome fraction co-eluting with salts ill size-exclusion chromatography allowed the separation of nine selenium species (excluding isomers and selenate) as monitored by inductively Coupled plasma mass spectrometry (ICP MS). The individual fractions were analyzed by electrospray QTOF MS/MS and hybrid linear ion trap/Orbitrap MSn after sample introduction by reversed-phase nanoHPLC and by hydrophilic interaction LC (HILIC), respectively. Out of the nine detected species. eight were identified oil the basis of accurate mass measurements and collision induced dissociation/fragmentation information. Seven Se-species (selenohomolanthionine, gamma-Glu-selenocystathionine, 2,3-DHP-selenocystathionine, N-acetyl-selenocystathionine, 2,3-DHP-selenohomolanthionine Se-methyl-selenoglutathione, and 2,3-DHP-Se-methylselenocysteine) were reported for the first time in Se-rich yeast. five of them have never been reported in any biological sample before. [less ▲] Detailed reference viewed: 14 (1 ULg) |
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