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Fast Screening of Diol Impurities in Methoxy Poly(Ethylene Glycol)s (mPEG)s by Liquid Chromatography on Monolithic Silica Rods

1
Laboratory of Organic and Macromolecular Chemistry (IOMC), Friedrich Schiller University Jena, Humboldtstr. 10, 07743 Jena, Germany
2
Jena Center for Soft Matter (JCSM), Friedrich Schiller University Jena, Philosophenweg 7, 07743 Jena, Germany
3
Center for Sepsis Control and Care (CSCC), Jena University Hospital, Am Klinikum 1, 07747 Jena, Germany
*
Authors to whom correspondence should be addressed.
Polymers 2018, 10(12), 1395; https://doi.org/10.3390/polym10121395
Received: 30 November 2018 / Revised: 11 December 2018 / Accepted: 11 December 2018 / Published: 16 December 2018
(This article belongs to the Special Issue Hydrophilic Polymers)
The determination of diol impurities in methoxy poly(ethylene glycol)s (mPEG)s is of high importance, e.g., in the area of pharmaceutical applications, since mPEGs are considered the gold standard—based on properties of biocompatibility, stealth effect against the immune system, and well-established procedures used in PEGylation reactions. Herein, we communicate a straightforward and fast approach for the resolution of the PEGdiol impurities in mPEG products by liquid chromatography on reversed-phase monolithic silica-rods. Thus, we utilize fine, in-house prepared and narrow dispersity mPEGs (Ð ≤ 1.1) and commercial PEGdiol standards as a reference. Most efficient analysis of diol impurities becomes possible with reversed-phase liquid chromatography that results in selective elution of the PEGdiol from mPEG macromolecule populations in partition/adsorption mode. We do this by a minimum selectivity of the population of macromolecules characterizing the narrow molar mass distributions of mPEG. Control experiments with intentionally added water at the start of the well-controlled mPEG synthesis via the living anionic ring opening polymerization of ethylene oxide clearly reconciled the existence of PEGdiol impurity in chromatographed samples. The here-demonstrated methodology allows for the resolution of diol impurities of less than one percent in elution times of only a few minutes, confirmed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) of the collected elution fractions. The unique combination of the open flow-through pore structure of the monolithic silica rods and resultant varying accessibility of C18-derivatized pore surfaces indicates beneficial properties for robust and end-group-specific adsorption/partition liquid chromatography of synthetic macromolecules. View Full-Text
Keywords: anionic ring-opening polymerization; MALDI-TOF-MS; monolith; PEGdiol; pharmaceutical PEG; reversed-phase chromatography anionic ring-opening polymerization; MALDI-TOF-MS; monolith; PEGdiol; pharmaceutical PEG; reversed-phase chromatography
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Brunzel, M.; Majdanski, T.C.; Vitz, J.; Nischang, I.; Schubert, U.S. Fast Screening of Diol Impurities in Methoxy Poly(Ethylene Glycol)s (mPEG)s by Liquid Chromatography on Monolithic Silica Rods. Polymers 2018, 10, 1395.

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