High-resolution polymer high performance liquid chromatography: Application of a saw tooth gradient for the separation of various polymers

Autor: Bernhard Durner, Frank-Michael Matysik, Thomas Ehmann
Rok vydání: 2019
Předmět:
Zdroj: Journal of Chromatography A. 1587:88-100
ISSN: 0021-9673
DOI: 10.1016/j.chroma.2018.11.075
Popis: Currently, a lot of research effort in polymer analysis by liquid chromatographic techniques, including size exclusion chromatography (SEC), polymer HPLC or liquid chromatography at critical conditions, is done aiming to improve separation performance. In this study, novel gradient protocols were investigated primarily based on gradient polymer elution chromatography (GPEC). Starting with linear gradients and stepwise gradients a new periodic saw tooth gradient profile was developed and optimized. Optimum settings for the saw tooth gradient design were evaluated by design of experiments (DoE) based on Taguchi’s methodology for various types of stationary phases. The gain of peak resolution was dependent on the effective gradient step height. The optimized protocol enabled high-resolution polymer HPLC (HRP-HPLC) separations with common HPLC instruments. The quality of separation was evaluated by heart-cut fraction collection of HRP-HPLC and subsequent determination of the individual fractions by SEC or MALDI-ToF mass spectrometry. Finally, different types of polymers, such as PVC, PDMS, PMMA, or PPG, were studied with the new method and a universal applicability was shown.
Databáze: OpenAIRE