NMR Longitudinal Rotating Frame Relaxation Time (T) with a Weak Spin Locking Field as an Approach to Characterize Solid-State Active Pharmaceutical Ingredients: Proof of Concept.

Nuclear magnetic resonance (NMR) longitudinal rotating frame relaxation time (T), rarely used in low-field NMR, can be more effective than conventional T and T relaxation times to differentiate polymorphic forms of solid pharmaceuticals. This could be attributed to T sensibility to structural and molecular dynamics that can be enhanced by changing the strength of the oscillating magnetic field () of spinlock pulses. Here, we compared the capacity of T, T, and T to differentiate inactive (A) and active (C) crystalline forms of the World Health Organization essential drug Mebendazole.

Mechanically robust cationic cellulose nanofibril 3D scaffolds with tuneable biomimetic porosity for cell culture.

3D foam scaffolds were produced in a "bottom-up" approach from lyophilised cationic cellulose nanofibril (CCNF) dispersions and emulsions (CCNF degree of substitution 23.0 ± 0.9%), using a directional freezing/lyophilisation approach, producing internal architectures ranging from aligned smooth walled micro channels, mimicking vascularised tissue, to pumice-like wall textures, reminiscent of porous bone.

On resonance phase alternated CWFP sequences for rapid and simultaneous measurement of relaxation times.

T1 and T2 relaxation times have been frequently used as probes for physical-chemical properties in several time-domain NMR applications (TD-NMR) such as food, polymers and petroleum industries. T2 measurements are usually achieved using the traditional Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence because it is a fast and robust method. On the other hand, the traditional methods for determining T1, i.

Quantitative (13)C MultiCP solid-state NMR as a tool for evaluation of cellulose crystallinity index measured directly inside sugarcane biomass.

Background: The crystallinity index (CI) is often associated with changes in cellulose structure after biological and physicochemical pretreatments. While some results obtained with lignocellulosic biomass demonstrate a progressive increase in the CI as a function of pretreatments, it is also shown that the CI can significantly vary depending on the choice of the measurement method. Besides, the influence of the CI on the recalcitrance of biomass has been controversial for a long time, but the most recent results tend to point out that the efficiency of pretreatments in reducing the recalcitrance is not clearly correlated with the decrease of the CI.

A double-component Anderson-Weiss approach for describing NMR signals of mobile SIn units: application to constant-time DIPSHIFT experiments.

A composed Gaussian local field is proposed to describe the effect of molecular motions on NMR signals of SIn units (e.g., CHn or NHn), based upon the well-know Anderson-Weiss (AW) approximation.

Recoupled separated-local-field experiments and applications to study intermediate-regime molecular motions.

A specific separated-local-field NMR experiment, dubbed Dipolar-Chemical-Shift Correlation (DIPSHIFT) is frequently used to study molecular motions by probing reorientations through the changes in XH dipolar coupling and T₂. In systems where the coupling is weak or the reorientation angle is small, a recoupled variant of the DIPSHIFT experiment is applied, where the effective dipolar coupling is amplified by a REDOR-like π-pulse train. However, a previously described constant-time variant of this experiment is not sensitive to the motion-induced T₂ effect, which precludes the observation of motions over a large range of rates ranging from hundreds of Hz to around a MHz.

Correlation between molecular conformation, packing, and dynamics in oligofluorenes: a theoretical/experimental study.

Fluorene-based systems have shown great potential as components in organic electronics and optoelectronics (organic photovoltaics, OPVs, organic light emitting diodes, OLEDs, and organic transistors, OTFTs). These systems have drawn attention primarily because they exhibit strong blue emission associated with relatively good thermal stability. It is well-known that the electronic properties of polymers are directly related to the molecular conformations and chain packing of polymers.

Chemical and morphological characterization of sugarcane bagasse submitted to a delignification process for enhanced enzymatic digestibility.

Background: In recent years, biorefining of lignocellulosic biomass to produce multi-products such as ethanol and other biomaterials has become a dynamic research area. Pretreatment technologies that fractionate sugarcane bagasse are essential for the successful use of this feedstock in ethanol production. In this paper, we investigate modifications in the morphology and chemical composition of sugarcane bagasse submitted to a two-step treatment, using diluted acid followed by a delignification process with increasing sodium hydroxide concentrations.

Intermediate motions and dipolar couplings as studied by Lee-Goldburg cross-polarization NMR: Hartmann-Hahn matching profiles.

In this article, we evaluate the use of simple Lee-Goldburg cross-polarization (LG-CP) NMR experiments for obtaining quantitative information of molecular motion in the intermediate regime. In particular, we introduce the measurement of Hartmann-Hahn matching profiles for the assessment of heteronuclear dipolar couplings as well as dynamics as a reliable and robust alternative to the more common analysis of build-up curves. We have carried out dynamic spin dynamics simulations in order to test the method's sensitivity to intermediate motion and address its limitations concerning possible experimental imperfections.

Intermediate motions as studied by solid-state separated local field NMR experiments.

In this report, the application of a class of separated local field NMR experiments named dipolar chemical shift correlation (DIPSHIFT) for probing motions in the intermediate regime is discussed. Simple analytical procedures based on the Anderson-Weiss (AW) approximation are presented. In order to establish limits of validity of the AW based formulas, a comparison with spin dynamics simulations based on the solution of the stochastic Liouville-von-Neumann equation is presented.

CONTRA: improving the performance of dynamic investigations in natural abundance organic solids by mirror-symmetric constant-time CODEX.

We present a minor but essential modification to the CODEX 1D-MAS exchange experiment. The new CONTRA method, which requires minor changes of the original sequence only, has advantages over the previously introduced S-CODEX, since it is less sensitive to artefacts caused by finite pulse lengths. The performance of this variant, including the finite pulse effect, was confirmed by SIMPSON calculations and demonstrated on a number of dynamic systems.