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  • A simple HPLC-MS method for the quantitative determination of the composition of bacterial medium chain-length polyhydroxyalkanoates.

A simple HPLC-MS method for the quantitative determination of the composition of bacterial medium chain-length polyhydroxyalkanoates.

Journal of separation science (2008-05-08)
Andreas Grubelnik, Luzia Wiesli, Patrick Furrer, Daniel Rentsch, Roland Hany, Veronika R Meyer
RESUMEN

Bacterial poly(hydroxyalkanoates) (PHAs) vary in the composition of their monomeric units. Besides saturated side-chains, unsaturated ones can also be found. The latter leads to unwanted by-products (THF ester, secondary alcohols) during acidic cleavage of the polymer backbone in the conventional analytical assays. To prevent these problems, we developed a new method for the reductive depolymerization of medium chain-length PHAs, leading to monomeric diols that can be separated and quantified by HPLC/MS. Reduction is performed at room temperature with lithium aluminum hydride within 5-15 min. The new method is faster and simpler than the previous ones and is quantitative. The results are consistent with the ones obtained by quantitative (1)H NMR.

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Sigma-Aldrich
Lithium aluminum hydride solution, 1.0 M in THF
Sigma-Aldrich
Lithium aluminum hydride solution, 2.0 M in THF
Sigma-Aldrich
Lithium aluminum hydride solution, 1.0 M in diethyl ether
Sigma-Aldrich
Lithium aluminum hydride solution, 2.3 M in 2-methyltetrahydrofuran