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Feasibility of an on-line restricted access material/liquidchromatography/tandem mass spectrometry method in the rapid and sensitive determination of organophosphorustriesters in human blood plasma
Stockholm University, Faculty of Science, Department of Analytical Chemistry.
2003 (English)In: Journal of chromatography. B, ISSN 1570-0232, Vol. 795, no 2, 245-256 p.Article in journal (Refereed) Published
Abstract [en]

A rapid on-line solid phase extraction/liquid chromatography/tandem mass spectrometry (SPE/LC/MS/MS) method usingrestricted access material (RAM) was developed for the simultaneous determination of eight organophosphorus triesters inuntreated human blood plasma. In a process involving column-switching techniques, the analytes were enriched on the RAMcolumn, separated using a C-18 analytical column and detected with LC/MS. Tandem mass spectrometrywas used to characterizeand quantify the analytes. To elucidate the fragmentation pathway of a number of the analytes, MS3 experiments using an iontrap mass spectrometer were performed. The matrix effects associated with using APCI and ESI interfaces were investigated.The recoveries obtained were in the range 60–92% (R.S.D. < 6%), with estimated detection limits between 0.2 and 1.8 ng/mlof plasma, and the total analysis time was 27 min.

Place, publisher, year, edition, pages
2003. Vol. 795, no 2, 245-256 p.
URN: urn:nbn:se:su:diva-38259DOI: 10.1016/S1570-0232(03)00568-3OAI: diva2:308464
Available from: 2010-04-06 Created: 2010-04-06 Last updated: 2010-04-22Bibliographically approved
In thesis
1. Novel Solid Phase Extraction and Mass Spectrometry Approaches to Multicomponent Analyses in Complex Matrices
Open this publication in new window or tab >>Novel Solid Phase Extraction and Mass Spectrometry Approaches to Multicomponent Analyses in Complex Matrices
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Analysis of compounds present in complex matrices is always a challenge, which can be partly overcome by applying various sample preparation techniques prior to detection. Ideally, the extraction techniques should be as selective as possible, to minimize the concentration of interfering substances. In addition, results can be improved by efficient chromatographic separation of the sample components. The elimination of interfering substances is especially important when utilizing mass spectrometry (MS) as a detection technique since they influence the ionization yields. It is also important to optimize ionization methods in order to minimize detection limits.

In the work this thesis is based upon, selective solid phase extraction (SPE) materials, a restricted access material (RAM) and graphitized carbon black (GCB) were employed for clean up and/or pre-concentration of analytes in plasma, urine and agricultural drainage water prior to liquid chromatography/mass spectrometry (LC/MS). Two SPE formats, in which GCB was incorporated in µ-traps and disks, were developed for cleaning up small and large volume samples, respectively. In addition, techniques based on use of sub-2 µm C18 particles at elevated temperatures and a linear ion trap (LIT) mass spectrometer were developed to improve the efficiency of LC separation and sensitivity of detection of 6-formylindolo[3,2-b]carbazole (FICZ) metabolites in human urine.

It was also found that GCB can serve not only as a SPE sorbent, but also as a valuable surface for surface-assisted laser desorption ionization (SALDI) of small molecules. The dual functionality of GCB was utilized in a combined screening-identification/quantification procedure for fast elimination of negative samples. This may be particularly useful when processing large numbers of samples. SALDI analyses of small molecules was further investigated and improved by employing two kinds of new surfaces: oxidized GCB nanoparticles and silicon nitride.

Place, publisher, year, edition, pages
Stockholm: Department of Analytical Chemistry, Stockholm University, 2010. 62 p.
Sample preparation, SPE, RAM, GCB µ-trap, GCB disk, High temperature LC, LC/MS, ESI, APCI, Matrix effects, LIT-MS, SALDI, Sample screening, Oxidized GCB, Silicon nitride
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
urn:nbn:se:su:diva-38625 (URN)978-91-7447-050-5 (ISBN)
Public defence
2010-06-02, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 10:00 (English)
Available from: 2010-05-11 Created: 2010-04-22 Last updated: 2010-05-04Bibliographically approved

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