Issue 14, 2021

Expanding current applications and permitting the analysis of larger intact samples by means of a 7 mm CMP–NMR probe

Abstract

Comprehensive multiphase NMR combines the ability to study and differentiate all phases (solids, gels, and liquids) using a single NMR probe. The general goal of CMP–NMR is to study intact environmental and biological samples to better understand conformation, organization, association, and transfer between and across phases/interfaces that may be lost with conventional sample preparation such as drying or solubilization. To date, all CMP–NMR studies have used 4 mm probes and rotors. Here, a larger 7 mm probehead is introduced which provides ∼3 times the volume and ∼2.4 times the signal over a 4 mm version. This offers two main advantages: (1) the additional biomass reduces experiment time, making 13C detection at natural abundance more feasible; (2) it allows the analysis of larger samples that cannot fit within a 4 mm rotor. Chicken heart tissue and Hyalella azteca (freshwater shrimp) are used to demonstrate that phase-based spectral editing works with 7 mm rotors and that the additional biomass from the larger volumes allows detection with 13C at natural abundance. Additionally, a whole pomegranate seed berry (aril) and an intact softgel capsule of hydroxyzine hydrochloride are used to demonstrate the analysis of samples too large to fit inside a conventional 4 mm CMP probe. The 7 mm version introduced here extends the range of applications and sample types that can be studied and is recommended when 4 mm CMP probes cannot provide adequate signal-to-noise (S/N), or intact samples are simply too big for 4 mm rotors.

Graphical abstract: Expanding current applications and permitting the analysis of larger intact samples by means of a 7 mm CMP–NMR probe

Supplementary files

Article information

Article type
Paper
Submitted
06 Mae 2021
Accepted
08 Mezh. 2021
First published
10 Mezh. 2021

Analyst, 2021,146, 4461-4472

Expanding current applications and permitting the analysis of larger intact samples by means of a 7 mm CMP–NMR probe

P. Ning, D. Lane, R. Ghosh Biswas, A. Jenne, M. Bastawrous, R. Soong, D. Schmidig, T. Frei, P. De Castro, I. Kovacevic, S. Graf, S. Wegner, W. Bermel, F. Busse, T. Kuehn, R. Kuemmerle, J. Struppe, M. Fey, H. J. Stronks, M. Monette, M. J. Simpson and A. J. Simpson, Analyst, 2021, 146, 4461 DOI: 10.1039/D1AN00809A

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