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Coupled Liquid Separation and Spectrometric Detection of Organic Compounds Containing Hetero-atoms
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry, Analytical Chemistry.
2004 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis exemplifies the strength in the combination of inductively coupled plasma (ICP) spectrometry and electrospray ionization tandem mass spectrometry ESI-MS/MS as detection techniques for liquid chromatography (LC) in the search for and investigation of compounds that bind or can bind hetero-atoms. Furthermore, some aspects involved in the coupling of LC and ICP spectrometry and quantification without identical standards have been studied.

The importance of using a separation step in combination with ICP spectrometry was shown for urine and blood plasma samples from patients treated with boron neutron capture therapy. In addition to the carrier molecule used in the therapy, one major and a few possible minor metabolites were found in the urine samples. One fragment mass of the major metabolite was obtained with LC-ESI-MS/MS. Liquid chromatography coupled to ICP-MS was also shown to be a valuable tool for fingerprinting metal-binding compounds in complex matrices, such as siderophores (iron-complexing compounds) in soil. The presence of at least two siderophores in a field soil solution sample could be revealed by LC-ICP-MS. Their identities could thereafter be determined by LC-ESI-MS/MS.

The non-UV-absorbing o-carboranylalanine could be quantified in relation to its degradation products by LC-ICP-AES, which provided information about the mechanism behind the degradation. Moreover, LC-ICP spectrometry was shown to provide an accurate quantification of biomolecules (bias < 10 %) when evaluated from external calibration graphs based on inorganic elemental standards.

Finally, the causes of the large decrease in boron signal seen when adding acetonitrile to the LC mobile phase in LC-ICP-MS was investigated in some detail. Space charge effects might explain a large part of the depression from carbon species on the boron signal.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis , 2004. , p. 47
Series
Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1104-232X ; 933
Keyword [en]
Analytical chemistry
Keyword [sv]
Analytisk kemi
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-3977ISBN: 91-554-5863-7 (print)OAI: oai:DiVA.org:uu-3977DiVA, id: diva2:164007
Public defence
2004-02-27, B42, BMC, Husargatan 3, Uppsala, 10:15
Opponent
Supervisors
Available from: 2004-01-30 Created: 2004-01-30 Last updated: 2013-09-24Bibliographically approved
List of papers
1. Determination of boron containing compounds in urine and blood plasma from boron neutron capture therapy patients: The importance of using coupled techniques
Open this publication in new window or tab >>Determination of boron containing compounds in urine and blood plasma from boron neutron capture therapy patients: The importance of using coupled techniques
2002 In: Anal. Chem., Vol. 74, no 20, p. 5358-5363Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-91312 (URN)
Available from: 2004-01-30 Created: 2004-01-30Bibliographically approved
2. Fingerprinting metal-containing biomolecules after reductive displacement of iron by gallium and subsequent column-switched LC-ICPMS analysis applied on siderophores
Open this publication in new window or tab >>Fingerprinting metal-containing biomolecules after reductive displacement of iron by gallium and subsequent column-switched LC-ICPMS analysis applied on siderophores
Show others...
2004 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 76, no 9, p. 2618-2622Article in journal (Refereed) Published
Abstract [en]

Column-switching liquid chromatography followed by low-resolution ICPMS was evaluated as a tool for speciation analysis of metal-containing biomolecules. The strategy was applied on siderophores, strong iron chelators of low molecular weight (M(w) < 1500). Prior to the LC-ICPMS analysis, reductive displacement of iron by gallium was performed using ascorbate as the reducing agent to increase the sensitivity. Different experimental conditions during the exchange reaction were tested using ferrichrysin and ferrichrome for evaluation. A reaction time of 30 min and a pH of 3.9 gave an exchange yield of 27 and 83% for ferrichrysin and ferrichrome, respectively. A gradient elution profile was also developed to separate gallium-chelated siderophores on a PGC column. Detection limits for standard solutions of ferrichrysin and ferrichrome in the low-nanomolar range were obtained by monitoring the gallium-69 isotope. The combined use of LC-ICPMS and LC-ESI-MS/MS was also evaluated as a tool to identify unknown metal complexes, here siderophores, in field soil solution samples.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:uu:diva-94665 (URN)10.1021/ac0355000 (DOI)15117206 (PubMedID)
Available from: 2006-08-30 Created: 2006-08-30 Last updated: 2017-12-14Bibliographically approved
3. A kinetic study of the self-degradation of o-carboranylalanine to nido-carboranylalanine in solution
Open this publication in new window or tab >>A kinetic study of the self-degradation of o-carboranylalanine to nido-carboranylalanine in solution
Show others...
1999 In: Acta Chem. Scand., Vol. 53, no 9, p. 731-736Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-91314 (URN)
Available from: 2004-01-30 Created: 2004-01-30Bibliographically approved
4. The use of inorganic elemental standards in the quantification of proteins and biomolecular compounds by inductively coupled plasma spectrometry
Open this publication in new window or tab >>The use of inorganic elemental standards in the quantification of proteins and biomolecular compounds by inductively coupled plasma spectrometry
2002 In: J. Anal. At. Spectrom, Vol. 17, no 5, p. 491-496Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-91315 (URN)
Available from: 2004-01-30 Created: 2004-01-30Bibliographically approved
5. Matrix effects of organic solvents in the determination of boron containing compounds by ICP-MS
Open this publication in new window or tab >>Matrix effects of organic solvents in the determination of boron containing compounds by ICP-MS
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Manuscript (Other academic)
Identifiers
urn:nbn:se:uu:diva-91316 (URN)
Available from: 2004-01-30 Created: 2004-01-30 Last updated: 2010-01-13Bibliographically approved

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