Comprehensive Multiphase NMR Probehead with Reduced Radiofrequency Heating Improves the Analysis of Living Organisms and Heat-Sensitive Samples

• Published in: Analytical chemistry (Washington) 2021-07, Vol.93 (29), p.10326-10333
• Main Authors: Ning, Paris, Lane, Daniel, Ghosh Biswas, Rajshree, Soong, Ronald, Schmidig, Daniel, Frei, Thomas, De Castro, Peter, Kovacevic, Ivan, Graf, Stephan, Wegner, Sebastian, Busse, Falko, Kuehn, Till, Struppe, Jochem, Fey, Michael, Stronks, Henry J, Monette, Martine, Simpson, Myrna J, Simpson, André J
• Format: Article
• Language: English
• Subjects: Aquatic organisms; Chemical speciation; Chemistry; Decoupling; In vivo methods and tests; Multiphase; NMR; Nuclear magnetic resonance; Organisms; Phases; Probes; Radio frequency heating; Saline solutions; Salts; Shellfish; Solenoids
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/acs.analchem.1c01932

Comprehensive multiphase (CMP) NMR, first described in 2012, combines all of the hardware components necessary to analyze all phases (solid, gel, and solution) in samples in their natural state. In combination with spectral editing experiments, it can fully differentiate phases and study the transfer of chemical species across and between phases, providing unprecedented molecular-level information in unaltered natural systems. However, many natural samples, such as swollen soils, plants, and small organisms, contain water, salts, and ionic compounds, making them electrically lossy and susceptible to RF heating, especially when using high-strength RF fields required to select the solid domains. While dedicated reduced-heating probes have been developed for solid-state NMR, to date, all CMP-NMR probes have been based on solenoid designs, which can lead to problematic sample heating. Here, a new prototype CMP probe was developed, incorporating a loop gap resonator (LGR) for decoupling. Temperature increases are monitored in salt solutions analogous to those in small aquatic organisms and then tested in vivo on Hyalella azteca (freshwater shrimp). In the standard CMP probe (solenoid), 80% of organisms died within 4 h under high-power decoupling, while in the LGR design, all organisms survived the entire test period of 12 h. The LGR design reduced heating by a factor of ∼3, which allowed 100 kHz decoupling to be applied to salty samples with generally ≤10 °C sample heating. In addition to expanding the potential for in vivo research, the ability to apply uncompromised high-power decoupling could be beneficial for multiphase samples containing true crystalline solids that require the strongest possible decoupling fields for optimal detection.