SPICY: a method for single scan rotating frame relaxometry

Tolkkinen, Katja; Mailhiot, Sarah; Selent, Anne; Mankinen, Otto; Henschel, H.; Nieminen, Miika T.; Hanni, Matti; Kantola, Anu Maria; Liimatainen, Timo; Telkki, Ville‐Veikko

doi:10.1039/d2cp05988f

Cited by 2 publications

References 74 publications

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Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules

Tolkkinen,

Mankinen,

Mailhiot

et al. 2024

Anal. Chem.

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Nuclear magnetic resonance (NMR) relaxation times provide detailed information about molecular motions and local chemical environments. Longitudinal T 1 relaxation time is most often sensitive to relatively fast, nano-to picosecond ranges of molecular motion. Rotating frame T 1ρ relaxation time reflects a much slower, micro-to millisecond range of motion, and the motional regime can be tuned by changing spin-lock field strength. Conventional methods for measuring T 1 and T 1ρ relaxation times are time-consuming, since experiments must be repeated many times with incremented magnetization recovery or decay delay. In this work, we introduce two novel and efficient NMR methods to correlate the T 1 and T 1ρ relaxation times. The first method, IR-SPICY, combines the conventional T 1 inversion recovery (IR) with the single-scan T 1ρ detection-based spin-lock cycle (SPICY). The second method, ultrafast (UF) IR-SPICY, allows measurement of whole two-dimensional T 1 −T 1ρ correlation data in a single scan, in a couple of seconds, based on spatial encoding of the T 1 dimension. We demonstrate the performance of the methods by studying relaxation of water in porous silica and hydrogel samples, latter acting as a model of the articular cartilage extracellular matrix. The methods allow correlating different molecular motional regimes, potentially providing unprecedented information about various chemical and biochemical systems, such as structures and fluid dynamics in porous materials, macromolecular changes in tissues, and protein dynamics. One to three orders of magnitude shortened experiment time enable the studies of changing or degrading samples. Furthermore, the single-scan approach may significantly facilitate the use of modern nuclear-spin hyperpolarization techniques to enhance the sensitivity of T 1 −T 1ρ measurements by several orders of magnitude.

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Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules

Tolkkinen,

Mankinen,

Mailhiot

et al. 2024

Anal. Chem.

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Nuclear spin relaxation

Tayler

2024

Nuclear Magnetic Resonance

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This chapter explores current theoretical and experimental trends in nuclear spin relaxation, providing a digest of around 100 research papers published between 2022 and mid 2023. As is customary, this deliberately excludes the latest literature to capture trends and insights that have developed after publication. Throughout, emphasis is placed on a few topics: (1) relaxation in systems that exhibit enhanced nuclear spin polarization, through techniques like dynamic nuclear polarization and parahydrogen-induced polarization that have revolutionized signal-to-noise ratios in NMR and MRI; (2) relaxation in liquids at low and ultralow magnetic fields, where interest is drawn towards new mechanisms and applications in biomolecular systems; (3) long-lived spin states, a relaxation methodology that is complementary to the usual T1 and T2 approaches, which always seems to be applied in molecules with increasing complexity and relevance to biochemistry. Conventional study areas are also reviewed, grouped by phase of matter (solid, liquid, gas, mixtures) and technique (theory/modeling, experiment: solvent-relaxation, co-solute relaxation, relaxation-dispersion mapping, and fast-field cycling).

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SPICY: a method for single scan rotating frame relaxometry

Abstract: T_1ρ is an NMR relaxation mode which is sensitive to low frequency molecular motions, making it an especially valuable tool in biomolecular research. Here, we introduce a new method, SPICY,...

Cited by 2 publications

References 74 publications

Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules

Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules

Nuclear spin relaxation

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SPICY: a method for single scan rotating frame relaxometry

Abstract: T_1ρ is an NMR relaxation mode which is sensitive to low frequency molecular motions, making it an especially valuable tool in biomolecular research. Here, we introduce a new method, SPICY,...

Cited by 2 publications

References 74 publications

Ultrafast T1–T1ρ NMR for Correlating Different Motional Regimes of Molecules

Ultrafast T1–T1ρ NMR for Correlating Different Motional Regimes of Molecules

Nuclear spin relaxation

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Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules

Ultrafast T₁–T_1ρ NMR for Correlating Different Motional Regimes of Molecules