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Diffusion ordered  NMR spectroscopy  application  to medicines control and research  

Lech Kozerski 1,2Elżbieta Bednarek 2Jerzy Sitkowski 1,2Wojciech Bocian 1,2Robert Kawęcki 1

1. Polish Academy of Science, Institute of Organic Chemistry, Kasprzaka 44/52, Warszawa 01-224, Poland
2. National Medicines Institut (NIL), Chełmska 30/34, Warsaw 00-725, Poland


DOSY  NMR  (Diffusion Ordered Spectroscopy) is a powerful method to analyse the mixtures of chemical species in solution.1 ( and references therein)  It relies on measurement of translational diffusion coefficients, Dt  x 10-10 [ m2/s ] for species in solution. Each spectral line in 1H NMR spectrum of a given chemical entity is characterised by the same Dt , providing the line is separated from spectral lines of other substance in solution. The larger difference in MW of the two species , the larger the difference in Dt coefficients between them.  Separation of lines is better achieved with higher magnetic fields. Large molecules diffuse much slowly than smaller ones.

The lecture will cover the title topics chosen from authors’ research and drug control activity.

This, inter alia, applies to:

 1. Differentiating between oligomers of proteins (insulin) 2

 2. Establishing  medicines binding to biomolecules ( topotecan) TPT 3

 3. Differentiating between OSCS impurity of ca.18-20 kDa  MW range with

      LMWH  of ca.6 - 8 kDa range or unfractioned heparins.

The results concerning first Ph.Eur. monograph on heparin identity test by 1H NMR will be presented.

1. Nilsson M., Gil A.M. Dellagillo I, Morris G.A. Anal. Chem. 2004, 76,  5418-5422

2. W. Bocian, J. Sitkowski , A. Tarnowska,  E. Bednarek, R. Kawęcki, W. Koźmiński, L. Kozerski  Proteins, Struct. Funct. Bioinformatics    2008 71 1057-1065

3.  W. Bocian, E. Bednarek, J. Sitkowski, R. Kawęcki,  M.P. Williamson, P.E. Hansen , L. Kozerski Chem. Eur. J2008  14(9)  2788-2794.

4.  I. McEwen, B. Mulloy, E. Hellwig, L. Kozerski, T. Beyer, U. Holzgrabe, A. Rodomonte, R. Wanko, J-M. Spieser  Pharmeuropa Bio  2008-1 31-39.



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Related papers

Presentation: Oral at VII Multidyscyplinarna Konferencja Nauki o Leku, by Lech Kozerski
See On-line Journal of VII Multidyscyplinarna Konferencja Nauki o Leku

Submitted: 2010-02-23 15:55
Revised:   2010-02-24 16:38