NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization

Jacqueline L. Pasek-Allen; Randall K. Wilharm; John C. Bischof; Valérie C. Pierre

doi:10.1021/ACSOMEGA.2C07669

NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization

Jacqueline L. Pasek-Allen, Randall K. Wilharm, John C. Bischof, Valérie C. Pierre

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Abstract

The molecular weight, purity, and functionalization of polyethylene glycols are often characterized by ¹H NMR spectroscopy. Oft-forgotten, the typical ¹H NMR pulse sequence is not ¹³C decoupled. Hence, for large polymers, the ¹³C coupled ¹H peaks arising from the repeating units have integrations comparable to that of the ¹H of the terminal groups. Ignoring this coupling leads to erroneous assignments. Once correctly assigned, these ¹³C coupled ¹H peaks can be used to determine both the molecular weight of the polymer and the efficacy of conjugation of a terminal moiety more accurately than the uncoupled ¹H of the repeating unit.

Original language	English (US)
Pages (from-to)	4331-4336
Number of pages	6
Journal	ACS Omega
Volume	8
Issue number	4
DOIs	https://doi.org/10.1021/ACSOMEGA.2C07669
State	Published - Jan 31 2023

Bibliographical note

Funding Information:
The authors thank Dr. Peter Flynn at the University of Utah, and Dr. Todd Rappe and Dr. Letitia Yao at the University of Minnesota for useful discussions. This work was supported by 5 F31 DK124968-02, NSF EEC 1941543, R01 HL135046, DK124333, and R01 DK117425. Research reported in this publication was supported by the Office of the Vice President of Research, College of Science and Engineering at the University of Minnesota.

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© 2023 The Authors. Published by American Chemical Society.

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@article{f17c498fd5c543f29a3b830992710cd4,

title = "NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization",

abstract = "The molecular weight, purity, and functionalization of polyethylene glycols are often characterized by 1H NMR spectroscopy. Oft-forgotten, the typical 1H NMR pulse sequence is not 13C decoupled. Hence, for large polymers, the 13C coupled 1H peaks arising from the repeating units have integrations comparable to that of the 1H of the terminal groups. Ignoring this coupling leads to erroneous assignments. Once correctly assigned, these 13C coupled 1H peaks can be used to determine both the molecular weight of the polymer and the efficacy of conjugation of a terminal moiety more accurately than the uncoupled 1H of the repeating unit.",

author = "Pasek-Allen, {Jacqueline L.} and Wilharm, {Randall K.} and Bischof, {John C.} and Pierre, {Val{\'e}rie C.}",

note = "Funding Information: The authors thank Dr. Peter Flynn at the University of Utah, and Dr. Todd Rappe and Dr. Letitia Yao at the University of Minnesota for useful discussions. This work was supported by 5 F31 DK124968-02, NSF EEC 1941543, R01 HL135046, DK124333, and R01 DK117425. Research reported in this publication was supported by the Office of the Vice President of Research, College of Science and Engineering at the University of Minnesota. Publisher Copyright: {\textcopyright} 2023 The Authors. Published by American Chemical Society.",

year = "2023",

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language = "English (US)",

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T1 - NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization

AU - Pasek-Allen, Jacqueline L.

AU - Wilharm, Randall K.

AU - Bischof, John C.

AU - Pierre, Valérie C.

N1 - Funding Information: The authors thank Dr. Peter Flynn at the University of Utah, and Dr. Todd Rappe and Dr. Letitia Yao at the University of Minnesota for useful discussions. This work was supported by 5 F31 DK124968-02, NSF EEC 1941543, R01 HL135046, DK124333, and R01 DK117425. Research reported in this publication was supported by the Office of the Vice President of Research, College of Science and Engineering at the University of Minnesota. Publisher Copyright: © 2023 The Authors. Published by American Chemical Society.

PY - 2023/1/31

Y1 - 2023/1/31

N2 - The molecular weight, purity, and functionalization of polyethylene glycols are often characterized by 1H NMR spectroscopy. Oft-forgotten, the typical 1H NMR pulse sequence is not 13C decoupled. Hence, for large polymers, the 13C coupled 1H peaks arising from the repeating units have integrations comparable to that of the 1H of the terminal groups. Ignoring this coupling leads to erroneous assignments. Once correctly assigned, these 13C coupled 1H peaks can be used to determine both the molecular weight of the polymer and the efficacy of conjugation of a terminal moiety more accurately than the uncoupled 1H of the repeating unit.

AB - The molecular weight, purity, and functionalization of polyethylene glycols are often characterized by 1H NMR spectroscopy. Oft-forgotten, the typical 1H NMR pulse sequence is not 13C decoupled. Hence, for large polymers, the 13C coupled 1H peaks arising from the repeating units have integrations comparable to that of the 1H of the terminal groups. Ignoring this coupling leads to erroneous assignments. Once correctly assigned, these 13C coupled 1H peaks can be used to determine both the molecular weight of the polymer and the efficacy of conjugation of a terminal moiety more accurately than the uncoupled 1H of the repeating unit.

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JO - ACS Omega

JF - ACS Omega

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NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization

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NMR Characterization of Polyethylene Glycol Conjugates for Nanoparticle Functionalization

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