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SALDI-MS Method Development for Analysis of Pharmaceuticals and Polymer Degradation Products
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Polymer Technology. (Fiber- och polymervetenskap)
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 [en]
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: urn:nbn:se:kth:diva-91472ISBN: 978-91-7501-252-0 (print)OAI: oai:DiVA.org:kth-91472DiVA: diva2:510404
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
List of papers
1. Nanocomposites as novel surfaces for laser desorption ionization mass spectrometry
Open this publication in new window or tab >>Nanocomposites as novel surfaces for laser desorption ionization mass spectrometry
2011 (English)In: Analytical Methods, ISSN 1759-9660, E-ISSN 1759-9679, Vol. 3, no 1, 192-197 p.Article in journal (Refereed) Published
Abstract [en]

The possibility to utilize nanocomposite films as easy-to-handle surfaces for surface assisted laser desorption ionization-mass spectrometry (SALDI-MS) of small molecules, such as pharmaceutical compounds, was evaluated. The signal-to-noise values of acebutolol, propranolol and carbamazepine obtained on the nanocomposite surfaces were higher than the values obtained on plain PLA surface showing that the nanoparticles participate in the ionization/desorption process even when they are immobilized in the polymer matrix. The advantages of nanocomposite films compared to the free nanoparticles used in earlier studies are the ease of handling and reduction of instrument contamination since the particles are immobilized into the polymer matrix. Eight inorganic nanoparticles, titanium dioxide, silicon dioxide, magnesium oxide, hydroxyapatite, montmorillonite nanoclay, halloysite nanoclay, silicon nitride and graphitized carbon black at different concentrations were solution casted to films with polylactide (PLA). There were large differences in signal intensities depending on the type of drug, type of nanoparticle and the concentration of nanoparticles. Polylactide with 10% titanium oxide or 10% silicon nitride functioned best as SALDI-MS surfaces. The limit of detection (LOD) for the study was ranging from 1.7 ppm up to 56.3 ppm and the signal to noise relative standard deviations for the surface containing 10% silicon nitride was approximately 20-30%. Scanning electron microscopy demonstrated in most cases a good distribution of the nanoparticles in the polymer matrix and contact angle measurements showed increasing hydrophobicity when the nanoparticle concentration was increased, which could influence the desorption and ionization. Overall, the results show that nanocomposite films have potential as surfaces for SALDI-MS analysis of small molecules.

Keyword
SMALL-MOLECULE ANALYSIS, SALDI-MS, ORGANIC-COMPOUNDS, MATRIX, NANOPARTICLES, PEPTIDES, PROTEINS
National Category
Polymer Technologies Polymer Chemistry Analytical Chemistry
Identifiers
urn:nbn:se:kth:diva-31390 (URN)10.1039/c0ay00531b (DOI)000287294200027 ()2-s2.0-79952965109 (Scopus ID)
Note
QC 20110314Available from: 2011-03-14 Created: 2011-03-14 Last updated: 2017-12-11Bibliographically approved
2. Surface Assisted Laser Desorption Ionization-Mass Spectrometry (SALDI-MS) for Analysis of Polyester Degradation Products
Open this publication in new window or tab >>Surface Assisted Laser Desorption Ionization-Mass Spectrometry (SALDI-MS) for Analysis of Polyester Degradation Products
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.

Keyword
surface assisted laser desorption ionization-mass spectrometry (SALDI-MS), polyester, polycaprolactone, degradation, nanoparticles
National Category
Polymer Technologies Polymer Chemistry Analytical Chemistry
Identifiers
urn:nbn:se:kth:diva-91483 (URN)10.1007/s13361-012-0360-8 (DOI)000303685800010 ()2-s2.0-84864866736 (Scopus ID)
Note

Updated from submitted to published. QC 20120607

Available from: 2012-03-16 Created: 2012-03-16 Last updated: 2017-12-07Bibliographically approved

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