Mass spectrometry based identification of geometric isomers during metabolic stability study of a new cytotoxic sulfonamide derivatives supported by quantitative structure-retention relationships

PLoS One. 2014 Jun 3;9(6):e98096. doi: 10.1371/journal.pone.0098096. eCollection 2014.

Abstract

A set of 15 new sulphonamide derivatives, presenting antitumor activity have been subjected to a metabolic stability study. The results showed that besides products of biotransformation, some additional peaks occurred in chromatograms. Tandem mass spectrometry revealed the same mass and fragmentation pathway, suggesting that geometric isomerization occurred. Thus, to support this hypothesis, quantitative structure-retention relationships were applied. Human liver microsomes were used as an in vitro model of metabolism. The biotransformation reactions were tracked by liquid chromatography assay and additionally, fragmentation mass spectra were recorded. In silico molecular modeling at a semi-empirical level was conducted as a starting point for molecular descriptor calculations. A quantitative structure-retention relationship model was built applying multiple linear regression based on selected three-dimensional descriptors. The studied compounds revealed high metabolic stability, with a tendency to form hydroxylated biotransformation products. However, significant chemical instability in conditions simulating human body fluids was noticed. According to literature and MS data geometrical isomerization was suggested. The developed in sillico model was able to describe the relationship between the geometry of isomer pairs and their chromatographic retention properties, thus it supported the hypothesis that the observed pairs of peaks are most likely geometric isomers. However, extensive structural investigations are needed to fully identify isomers' geometry. An effort to describe MS fragmentation pathways of novel chemical structures is often not enough to propose structures of potent metabolites and products of other chemical reactions that can be observed in compound solutions at early drug discovery studies. The results indicate that the relatively non-expensive and not time- and labor-consuming in sillico approach could be a good supportive tool assisting the identification of cis-trans isomers based on retention data. This methodology can be helpful during the structural identification of biotransformation and degradation products of new chemical entities--potential new drugs.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Biotransformation / drug effects
  • Cell Death / drug effects
  • Chromatography, Liquid
  • Humans
  • Isomerism
  • Mass Spectrometry*
  • Microsomes, Liver / metabolism
  • Models, Molecular
  • Software
  • Structure-Activity Relationship
  • Sulfonamides / chemistry*
  • Sulfonamides / metabolism*
  • Sulfonamides / toxicity

Substances

  • Sulfonamides

Grants and funding

The project was funded by the Polish National Science Centre granted under decision no. UMO-2011/01/N/NZ1/00214 and UMO-2011/03/B/NZ1/03113. M.B has obtained funding for the preparation of a doctoral dissertation from the National Science Centre under decision no. UMO-2013/08/T/NZ1/00764. This research work was supported by the system project “InnoDoktorant – Scholarships for PhD students, Vth edition”. The project was co-financed by the European Union in the frame of the European Social Fund supported by funds obtained from the quality-promoting subsidy under the KNOW programme 2012 – 2017. The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.