Platzhalter für Bild, Bild auf Titelfolie hinter das Logo einsetzen Sheetal Gangula, Institute of Food chemistry Quantitative analysis of complex oligomeric.

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Platzhalter für Bild, Bild auf Titelfolie hinter das Logo einsetzen Sheetal Gangula, Institute of Food chemistry Quantitative analysis of complex oligomeric mixtures by MS

8 May 2014 | Sheetal Gangula |TU Braunschweig 2 WHAT Distribution of substituents along the polymer chain o random distribution? o high and low substituted areas? WHY structure-property relationships o E.g. thermo-reversible gelation HOW quantitative mass spectrometry (MS) of oligomers Quantitative Analysis of Cellulose Ethers

8 May 2014 | Sheetal Gangula |TU Braunschweig 3 Quantitative MS of Methyl Cellulose methyl cellulose CH 3 CD 3 permethylation with CD 3 I partial degradation to oligomers mass spectrometric analysis R. Adden et al., Macromol. Chem. Phys., 207 (2006) number of [M+Na] +

8 May 2014 | Sheetal Gangula |TU Braunschweig Analysis by MS QUALITATIVE ANALYSIS Peak Identified by m/z value QUANTITATIVE ANALYSIS Depends on peak intensity But this is not simple as peak intensity varies depending on chemistry,instrumental parameters and mass differnce 4

8 May 2014 | Sheetal Gangula |TU Braunschweig For example different compounds at equimolar concentrations give different peak intensities Analysis by MS So for quantitative evaluation behaviour of different compounds with respect to chemistry and instrumental parameters has to be studied Mass spectrum from ESI-IT-MS m/z- DP2-Me DP2-Et The samples are seen as sodium adducts M+Na + in MS 5

8 May 2014 | Sheetal Gangula |TU Braunschweig Our current study preparation of a roughly equimolar oligosaccharide mixtures determination of the exact composition Evaluation of sodium adducts in mass spectrum ESI-IT MSMALDI-ToF-MS Samples measured under defined conditions 6

8 May 2014 | Sheetal Gangula |TU Braunschweig Sample Preparation 2,3,6-O-Me-β-CD 2,3,6-O-Med 3 -β-CD2,3,6-O-Et-β-CD Reductive amination Mixture of oligosaccharides (DP1-DP7) are obtainted from each sample Mixture of oligosaccharides (DP1-DP7) after reductive amination LC/UV Partial hydrolysis 7

8 May 2014 | Sheetal Gangula |TU Braunschweig Types of mixtures Three types of mixtures are presented : Methylated and deuteromethylated oligomeric mixtures (Me,Med 3 ) Methylated and ethylated oligomeric mixtures (Me,Et) Deuteromethylated and ethylated oligomeric mixtures (Med 3, Et) 8

8 May 2014 | Sheetal Gangula |TU Braunschweig ESI-IT-MS (electrospary ionization mass spectrometry) 9

8 May 2014 | Sheetal Gangula |TU Braunschweig Results are expressed as relative ion intensities. This is obtained by dividing the intensity of one compound in mass spectra by another compound w.r.t a certain DP in a mixture. Me,Med 3 mixture Me,Et mixture Med 3, Et mixture Results from ESI-IT-MS 10

8 May 2014 | Sheetal Gangula |TU Braunschweig COST action FP1105 STSM MALDI-ToF-MS: Measurements were performed at: The institute of Polymer Technology at KTH Royal Institute of Technology, Stockholm Instrument used: Bruker Daltonics Ultraflex

8 May 2014 | Sheetal Gangula |TU Braunschweig MALDI-ToF-MS (matrix assisted laser desorption mass spectrometry) 11 sDHB

8 May 2014 | Sheetal Gangula |TU Braunschweig Selection of laser power Me,Et Me,Med 3 LP 40 % LP 45 % LP 50 % LP 55 % LP 60 % 12

8 May 2014 | Sheetal Gangula |TU Braunschweig Results from MALDI-ToF-MS DP2 Results are expressed as relative ion intensities. This is obtained by dividing the intensity of one compound in mass spectra by another compound w.r.t a certain DP in a mixture. Me,Med 3 mixture Me,Et mixture Med 3, Et mixture 13

8 May 2014 | Sheetal Gangula |TU Braunschweig SUMMARY Under optimal conditions for both instruments...  Me and Med 3 oligosaccharides are similar in polarities, hence their relative ion intensities in mass spectra are almost 1:1 with a little scattering for various DP. The scattering of data is lees in MALDI-ToF-MS compared to ESI-IT-MS.  Polarity of Et oligosaccharides is lower than that of Me-derivatives and Med 3 -derivatives, these compounds in ESI-IT-MS: show 3-4 times higher intensities, but this factor is decreasing with DP MALDI-ToF-MS: the factor is scattering around , but it has no clear trend. May be since there is difference in polarities of the compounds they may have different interaction with matrix so the scattering is higher. This has to be further investigated. 14

8 May 2014 | Sheetal Gangula |TU Braunschweig Thank you for your kind attention 15