uu.seUppsala University Publications
Change search
ReferencesLink to record
Permanent link

Direct link
Evaluation of sample preparation techniques for MALDI-TOF-MS analysis of oligosaccharides
Uppsala University, Disciplinary Domain of Medicine and Pharmacy, Faculty of Pharmacy, Department of Medicinal Chemistry, Analytical Pharmaceutical Chemistry.
2016 (English)Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
Abstract [en]

The aim of this study was to optimize the sample preparation and methods for analysis of oligosaccharides of hyaluronic acid with MALDI- TOF-MS. The analysis was carried out on an Autoflex speed MADLI-TOF- MS instrument with both linear and reflectron mode. Matrices used in this study were 2,5-DHB and Super-DHB and type of matrix was chosen depending on the size of the analyzed oligosaccharides. The application of sample and matrix on the target that gave the most homogenous crystallization was sandwich and the laser power in the MALDI was kept at 65 %. Since it is known that salts and buffers interfere with the analysis, sample clean-up such as solid phase extraction (SPE) in pipette tips and dialysis was performed. SPE worked best for low mass oligosaccharides and provided high intensity and little noise. With SPE a concentration of the analyte could be done which was the advantage over dialysis. Dialysis worked well for larger oligosaccharides and mixtures of different sized oligosaccharides. Another way of using MALDI for biomolecule analysis is with TLC-MALDI. A fast and accurate separation was achieved and analysis could be done directly from the plate. The optimized methods were evaluated according to linearity and precision, LOD, mass accuracy and matrix stability. The linearity and precision was good in a higher concentration range (50 μg/mL and higher), but the test for limit-of-detection (LOD) indicated that concentrations from 20-30 μg/mL could be analyzed with no interference from the background. The mass accuracy was within the acceptable limits according to Bruker Daltonics when a mass calibration was done for each analyzed sample. The stability of the matrix in solution was difficult to study because of the day-to-day variation in intensities given by the MALDI-TOF-MS technique. 

Place, publisher, year, edition, pages
2016. , 28 p.
UPTEC K, ISSN 1650-8297 ; 15037
Keyword [en]
Analytical Chemistry, MALDI-TOF-MS, Oligosaccharides
National Category
Pharmaceutical Chemistry
URN: urn:nbn:se:uu:diva-277957OAI: oai:DiVA.org:uu-277957DiVA: diva2:906040
External cooperation
Subject / course
Educational program
Master Programme in Chemical Engineering
Available from: 2016-08-23 Created: 2016-02-23 Last updated: 2016-08-23Bibliographically approved

Open Access in DiVA

fulltext(1151 kB)19 downloads
File information
File name FULLTEXT01.pdfFile size 1151 kBChecksum SHA-512
Type fulltextMimetype application/pdf

By organisation
Analytical Pharmaceutical Chemistry
Pharmaceutical Chemistry

Search outside of DiVA

GoogleGoogle Scholar
Total: 19 downloads
The number of downloads is the sum of all downloads of full texts. It may include eg previous versions that are now no longer available

Total: 10 hits
ReferencesLink to record
Permanent link

Direct link