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Surface Assisted Laser Desorption Ionization-Mass Spectrometry (SALDI-MS) for Analysis of Polyester Degradation Products
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Polymer Technology.ORCID iD: 0000-0002-7790-8987
2012 (English)In: Journal of the American Society for Mass Spectrometry, ISSN 1044-0305, E-ISSN 1879-1123, Vol. 23, no 6, 1071-1076 p.Article in journal (Refereed) Published
Abstract [en]

Novel surface assisted laser desorption ionization-mass spectrometry (SALDI-MS) method was developed for rapid analysis of low molecular mass polyesters and their degradation products by laser desorption ionization-mass spectrometry. Three polycaprolactone materials were analyzed by the developed method before and after hydrolytic degradation. The signal-to-noise values obtained by SALDI-MS were 20-100 times higher compared with the ones obtained by using traditional MALDI-MS matrices. A clean background at low mass range and higher resolution was obtained by SALDI-MS. Different nanoparticle, cationizing agent, and solvent combinations were evaluated. Halloysite nanoclay and magnesium hydroxide showed the best potential as SALDI surfaces. The SALDI-MS spectrum of the polyester hydrolysis products was verified by ESI-MS. The developed SALDI-MS method possesses several advantages over existing methods for similar analyses.

Place, publisher, year, edition, pages
2012. Vol. 23, no 6, 1071-1076 p.
Keyword [en]
surface assisted laser desorption ionization-mass spectrometry (SALDI-MS), polyester, polycaprolactone, degradation, nanoparticles
National Category
Polymer Technologies Polymer Chemistry Analytical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-91483DOI: 10.1007/s13361-012-0360-8ISI: 000303685800010Scopus ID: 2-s2.0-84864866736OAI: oai:DiVA.org:kth-91483DiVA: diva2:510420
Note

Updated from submitted to published. QC 20120607

Available from: 2012-03-16 Created: 2012-03-16 Last updated: 2017-12-07Bibliographically approved
In thesis
1. SALDI-MS Method Development for Analysis of Pharmaceuticals and Polymer Degradation Products
Open this publication in new window or tab >>SALDI-MS Method Development for Analysis of Pharmaceuticals and Polymer Degradation Products
2012 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

Surface assisted laser desorption ionization-mass spectrometry (SALDI-MS) was evaluated as a new tool for analysis of polymer degradation products. A SALDI method was developed enabling rapid analysis of low molecular mass polyesters and their degradation products. In addition, the possibility to utilize nanocomposite films as easy-to-handle surfaces for analysis of pharmaceutical compounds was investigated.

Poly(ε-caprolactone) was used as a model compound for SALDI-MS method development. The signal-to-noise values obtained by SALDI-MS were 20 times higher compared to traditional matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) of the same samples with 2,5-dihydroxybenzoic acid as a matrix. Halloysite nanoclay and magnesium oxide showed best potential as surfaces and clean backgrounds in the low mass range were observed. The SALDI-MS method for the analysis of polyester degradation products was also verified by electrospray ionization-mass spectrometry (ESI-MS). An advantage over ESI-MS is the possibility to directly analyze degradation products in buffer solutions. Compared to gas chromatography-mass spectrometry (GC-MS) it is possible to analyze polar compounds and larger molecular mass ranges at the same time as  complicated extraction steps are avoided.

The possibility to use nanocomposite films as surfaces instead of free nanoparticles was evaluated by solution casting of poly(lactide) (PLA) films with eight inorganic nanoparticles. The S/N values of the pharmaceutical compounds, acebutolol, propranolol and carbamazepine, analyzed on the nanocomposite surfaces were higher than the values obtained on the surface of plain PLA showing that the nanoparticles participated in the ionization/desorption process even when they are immobilized. Beside the ease of handling, the risk for instrument contamination is reduced when nanocomposites are used instead of free nanoparticles. The signal intensities depended on the type of drug, type and concentration of nanoparticle. PLA with 10 % titanium oxide or 10 % silicon nitride functioned best as SALDI-MS surfaces.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2012. 33 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2012:5
Keyword
Surface assisted laser desorption ionization-mass spectrometry (SALDI-MS), polyester degradation products, pharmaceutical compounds, nanoparticles, nanocomposites.
National Category
Polymer Chemistry Polymer Technologies Analytical Chemistry
Identifiers
urn:nbn:se:kth:diva-91472 (URN)978-91-7501-252-0 (ISBN)
Presentation
2012-03-12, K2, KTH, Teknikringen 28, entréplan, Stockholm, 10:15 (English)
Opponent
Supervisors
Note
QC 20120316Available from: 2012-03-16 Created: 2012-03-16 Last updated: 2012-03-16Bibliographically approved
2. LDI-MS strategies for analysis of polymer degradation products, additives and drugs
Open this publication in new window or tab >>LDI-MS strategies for analysis of polymer degradation products, additives and drugs
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The advancement of mass spectrometry (MS) has been and continues to be a prominent analytical technique for highly accurate determination of analytes. The goal of this thesis was to develop new laser desorption ionization-mass spectrometric (LDI-MS) methods for analysis of polymer degradation products, additives and drugs. Modifications in the sample preparation were evaluated in the presence and absence of surface assisting materials. Various nanoparticles were evaluated as effective absorbents for energy transfer in the LDI procedure of the small molecules.

In paper I and II, LDI-MS methods were developed for following the progression of chemical reactions. First, the procedure to optimize microwave assisted hydrothermal degradation products of cellulose were analyzed; second, the synthesis of glucose hexanoate ester plasticizers was monitored as a function of reaction time. The LDI-MS method provided rapid detection for the elucidation of the chemical products and their relative ratios. In contrast, the electrospray ionization-mass spectrometry (ESI-MS) analysis produced a noisy spectrum primarily containing peaks from salt clusters. A surface assisted laser desorption ionization-mass spectrometry (SALDI-MS) method was developed in paper III enabling the identification of poly(e-caprolactone) and its degradation products by using nanoparticles as the substrate. Similar analysis by matrix assisted laser desorption ionization-mass spectrometry (MALDI-MS) was not as successful due to convolution of the analyte peaks with clusters released from the matrix. ESI-MS analysis verified the SALDI-MS method as comparable degradation product patterns were observed. Furthermore, the possibility of using polylactide based nanocomposites as surfaces in the analysis of drugs was evaluated in paper IV. An advantage was the ease of handling compared to the use of free nanoparticles. Paper V introduces the potential of direct examination of oxygen plasma modified parylene C surfaces by a LDI-MS methodology. 

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2014. 57 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2014:33
Keyword
laser desorption ionization-mass spectrometry (LDI-MS), surface, polymer degradation products, additive, drugs, nanoparticles, nanocomposites
National Category
Polymer Technologies
Research subject
Chemistry
Identifiers
urn:nbn:se:kth:diva-152647 (URN)978-91-7595-233-8 (ISBN)
Public defence
2014-10-24, Kollegiesalen, Brinellvägen 8, KTH, Stockholm, 09:00 (English)
Opponent
Supervisors
Note

QC  20141002

Available from: 2014-10-02 Created: 2014-09-30 Last updated: 2014-10-02Bibliographically approved

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