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Structure determination of hyperbranched polyester BOLTORN H40 by 1D- and 2D-NMR spectroscopy

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Abstract

Hyperbranched polyester BOLTORN H40 is a perspective core molecule for synthesis of biodegradable block copolymers for drug delivery systems. NMR spectroscopy is the key method to study molecular structure of BOLTORN H40; however, interpretation of the 1H-NMR spectrum is still ambiguous. To determine the polyester structure precisely, a combination of 1D and 2D-NMR methods (1H, 13C, TOCSY, HSQC, HMBC) was suggested. These methods allow detecting signals from hydroxyl groups, whose correlations are crucial for identification of different types of units. The proportions of the terminal, linear, and dendritic monomeric units in BOLTORN H40 polyester were estimated to be 31, 53, and 16%, respectively. The degree of branching of the polyester is 0.47. According to this value, BOLTORN H40 belongs to a family of hyperbranched polyesters capable of forming micellar nanocontainers. These properties are critical for further precise characterization of block copolymers for various drug delivery applications.

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Acknowledgements

We thank Dr. Elena Bazanova and the Language Training and Testing Centre for help in the preparation of the English version of the article. 1H and 13C NMR experiments were supported by President’s grant for young scientists (project MK-70.2021.1.3). Two-dimensional correlation NMR experiments were supported by the Russian Science Foundation (project 18-73-10079-P).

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Authors and Affiliations

  1. Moscow Institute of Physics and Technology (National Research University), Moscow, Russia, 117303

    Valeriya Shpotya, Alexander Perepukhov & Alexander Maksimychev

  2. National Research Center Kurchatov Institute, Moscow, Russia, 123182

    Vitaly Gomzyak, Nikita Sedush & Sergey Chvalun

  3. Lomonosov Institute of Fine Chemical Technologies, Russian Technological University (MIREA), Moscow, Russia, 119454

    Vitaly Gomzyak

  4. Enikolopov Institute of Synthetic Polymeric Materials Russian Academy of Sciences, Moscow, Russia, 117393

    Sergey Chvalun

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  1. Valeriya Shpotya
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  2. Alexander Perepukhov
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Correspondence to Valeriya Shpotya.

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Fig. 7
figure 7

COSY NMR spectrum of BOLTORN H40 in DMSO-d6

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Shpotya, V., Perepukhov, A., Maksimychev, A. et al. Structure determination of hyperbranched polyester BOLTORN H40 by 1D- and 2D-NMR spectroscopy. Polym. Bull. 80, 4523–4534 (2023). https://doi.org/10.1007/s00289-022-04274-3

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  • DOI: https://doi.org/10.1007/s00289-022-04274-3

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