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Feasible analytical protocol for residual polymers in culture medium after biodegradation testing

Abstract

The development of biodegradable polymers and their certification require an analytical method that is both reliable and practical. Although biochemical oxygen demand (BOD) testing remains a robust method for confirming polymer metabolism, it does not provide precise information about the residual compounds present during and after biodegradation. Moreover, direct analysis of these residues is challenging, particularly when seawater interferes with the analysis. In this study, we propose an extraction/chemical-structure–analysis/molecular-mass–analysis protocol as an enhanced analytical approach for investigating culture medium after BOD biodegradation testing in seawater. We conducted BOD biodegradation tests of poly(3-hydroxybutyrate-co-3-hydroxyvalerate), poly(ε-caprolactone), and poly(butylene succinate) in seawater. After testing, 1H NMR analysis of the extracts revealed the chemical structures of the residual polymers and enabled the assessment of NMR degradability, which aligned well with the BOD biodegradability trend. Additionally, molecular mass analysis revealed changes in the molecular mass, supporting the evaluation of the polymer chain scission. This study advances analytical methods in the field of biodegradable polymers.

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Acknowledgements

Yuya Tachibana is grateful for the financial support from the JSPS KAKENHI Grant-in-Aid for Scientific Research (C) (number 20K12233). Ken-ichi Kasuya is grateful for financial support from the New Energy and Industrial Technology Development Organization (NEDO), project code JPNP14004. NMR measurements were performed on an NM-ECS400 NMR spectrometer and a JNM-ECA600 NMR spectrometer (JEOL Ltd., Tokyo, Japan) at the Core facility Management and Technology Collaboration Center of Gunma University. Seawater was collected from the shore of the Japan Agency for Marine–Earth Science and Technology (JAMSTEC) facing Tokyo Bay, Japan.

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Correspondence to Yuya Tachibana or Ken-ichi Kasuya.

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Sawanaka, Y., Torii, J., Tachibana, Y. et al. Feasible analytical protocol for residual polymers in culture medium after biodegradation testing. Polym J (2026). https://doi.org/10.1038/s41428-026-01187-0

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