A New Chirally Organized Trifluoromethylanthrylmethanol Derivative and Its Application as Chiral Solvating Agent

ChemistrySelect Journal“A New Chirally Organized Trifluoromethylanthrylmethanol Derivative and Its Application as Chiral Solvating Agent” By Eva Monteagudo, Pere de March, Ángel Álvarez‐Larena and Albert Virgili. ChemistrySelect, 2017, 2, pp. 7362-7367 DOI:10.1002/slct.201701429

The synthesis and structure of 1,1′‐(((10,10’‐(1,1′‐binaphthalene)‐2,2′‐diylbis(oxy))bis(methylene))bis(anthracene‐10,9‐diyl))bis(2,2,2‐trifluoroethanol), 4, is reported. This compound owns both axial and central chirality allowing its use as a chiral solvating agent (CSA) for the enantiomeric composition determination of several mixtures of chiral aromatic alcohols and amines using NMR. The study of the resulting diastereoisomeric complexes was carried out by determining its stoichiometry and association binding constants.

Solid-State-NMR a useful tool for the characterization of Hydrogen Storage Composite System

In Situ Formation of TiB2 Nanoparticles for Enhanced Dehydrogenation/Hydrogenation Reaction Kinetics of LiBH4–MgH2 as a Reversible Solid-State Hydrogen Storage Composite System

Fahim Karimi* , María V. C. Riglos, Antonio Santoru , Armin Hoell, Vikram S. Raghuwanshi, Chiara Milanese, Nils Bergemann, Claudio Pistidda, Pau Nolis , Maria D. Baro, Gökhan Gizer, Thi-Thu Le, P. Klaus Pranzas, Martin Dornheim, Thomas Klassen, Andreas Schreyer, and Julián Puszkiel

J. Phys. Chem. C, Article ASAP
DOI: 10.1021/acs.jpcc.8b02258
Publication Date (Web): May 9, 2018
ABSTRACT:To enhance the dehydrogenation/rehydrogenation kinetic behavior of the LiBH4–MgH2 composite system, TiF4 is used as an additive. The effect of this additive on the hydride composite system has been studied by means of laboratory and advanced synchrotron techniques. Investigations on the synthesis and mechanism upon hydrogen interaction show that the addition of TiF4 to the LiBH4–MgH2 composite system during the milling procedure leads to the in situ formation of well-distributed nanosized TiB2 particles. These TiB2 nanoparticles act as nucleation agents for the formation of MgB2 upon dehydrogenation process of the hydride composite system. The effect of TiB2 nanoparticles is maintained upon cycling.

11th Workshop on Magnetic Resonance Spectroscopy and Imaging (MRI/MRS) Applied to Laboratory Animals

Workshop dates: June 25th – 28th, 2018
Registration deadline: June 10th, 2018
Registration:   online
Capacity: Workshop limited to 4 participants (first come, first served)
Contact person: Silvia Lope-Piedrafita, PhD (silvia.lope@uab.es)

This course combines a comprehensive series of lectures on the technology of Magnetic resonance spectroscopy and imaging (MRS/MRI) with hands-on laboratory sessions to provide practical demonstrations of key concepts and procedures for preclinical studies.

Whether you are considering MRI as a research tool in your lab or just would like to learn more about MRI, this workshop addresses practical aspects of experimental MRI with laboratory animals and provide valuable hands-on experience on a 7 Tesla Bruker BioSpec spectrometer.

See the workshop brochure for more information or contact Dr. Silvia Lope via email.

NEW BOOK RELEASE: “Preclinical MRI methods and protocols”

“Preclinical MRI: Methods and Protocols” by Maria Luisa Garcia Martin and Pilar Lopez Larrubia (Editors). Part of the Methods in Molecular Biology book series (MIMB, volume 1718). DOI: 10.1007/978-1-4939-7531-0.

This book was conceived with the idea of providing an update on a wide variety of preclinical MRI methods and protocols to help technicians and researchers interested in this technology. The basics of MRI physics are introduced, followed by chapters describing updated methodology and protocols for some standard and more advanced MRI techniques covering diffusion, perfusion, functional imaging, in-vivo spectroscopy (proton and heteronuclear), susceptibility contrast MRI… The book also contains some chapters where some applications of those methods are illustrated in animal models of several diseases including cancer, stroke and neurodegeneration. Protocols are described in a step-by-step approach, with interesting notes and tips at the end of each chapter, which -a priori- should allow the new worker to obtain successful results with the first attempt ;o) .

Recovering energy

As is tradition in Catalonia in February, the group of SeRMN got together to enjoy a Calçotada, eating the typical Calçots (a type of scallion or green onion) well combined with a “Porró” (is a traditional glass wine pitcher).

Simultaneous RCSA and RDC measurement

Isotropic/Anisotropic NMR Editing by Resolution-Enhanced NMR Spectroscopy by Núria Marcó,  R. R. Gil and Teodor Parella. ChemPhysChem 2018, DOI: 10.1002/cphc.201800094

Modern resolution-enhanced NMR techniques can monitor the in-situ discrimination of co-existing isotropic and anisotropic contributions of small molecules dissolved in weakly aligning PMMA/CDCl3 media. The simultaneous sign-sensitive determination of accurate Δδ(1H) and Δδ(13C) between isotropic and anisotropic signals,  and/or  1TCH and 1JCH coupling constants (and consequently 1H-13C RDCs and 1H/13C RCSAs) can be performed from spectral-aliased HSQC spectra.

Pulse Programs Code for Bruker:

Precise characterization of mycobacterial cell wall lipid PTTM

Molecule confirmation and structure characterization of pentatriacontatrienyl mycolate in Mycobacterium smegmatisby M. Llorens-Fons, E. Julián, M. Luquin and M. Pérez-Trujillo. Chemistry and Physics of Lipids, 2018, Accepted Manuscript. DOI: https://doi.org/10.1016/j.chemphyslip.2017.12.006

Mycobacterium smegmatis is often used to study the different components of mycobacterial cell wall. Mycolic acids are important components of mycobacterial cell wall that have been associated with virulence. Recently, a novel lipid containing mycolic acids has been described in M. smegmatis. However, some uncertainties regarding the structure of this molecule named mycolate ester wax have been reported. The objective of this work was to perform an in depth structural study of this molecule for its precise characterization. Using 1H and 13C NMR spectroscopy, the molecular structure of mycolate ester wax found in M. smegmatis has been elucidated. The characterization was complemented with MS analyses. This molecule is formed by a carbon chain with three methyl substituted olefinic units and a mycolate structure with trans double bonds and cis cyclopropane rings. The present molecular study will facilitate the detection and identification of pentatriacontatrienyl mycolate (PTTM) in future studies by the performance of a simple 1D 1H NMR experiment.

Assessment of biodistribution using mesenchymal stromal cells

“Assessment of biodistribution using mesenchymal stromal cells: Algorithm for study design and challenges in detection methodologies” by Reyes B, Coca MI, Codinach M, López-Lucas MD, Del Mazo-Barbara A, Caminal M, Oliver-Vila I, Cabañas V, S. Lope-Piedrafita, García-López J, Moraleda JM, Fontecha CG, Vives J. Cytotherapy. 2017 :1060-1069. doi: 10.1016/j.jcyt.2017.06.004.

Biodistribution of candidate cell-based therapeutics is a critical safety concern that must be addressed in the preclinical development program. We aimed to design a decision tree based on a series of studies included in actual dossiers approved by competent regulatory authorities, noting that the design, execution and interpretation of pharmacokinetics studies using this type of therapy is not straightforward and presents a challenge for both developers and regulators. This work contributes to the standardization in the design of biodistribution studies by improving methods for accurate assessment of safety.

Eight studies were evaluated for the definition of a decision tree, in which mesenchymal stromal cells (MSCs) were administered to mouse, rat and sheep models using diverse routes (local or systemic), cell labeling (chemical or genetic) and detection methodologies (polymerase chain reaction (PCR), immunohistochemistry (IHC), fluorescence bioimaging, and magnetic resonance imaging (MRI). Moreover, labeling and detection methodologies were compared in terms of cost, throughput, speed, sensitivity and specificity.

Multiplicity-edited 1H-1H TOCSY experiment

Pau Nolis and Teodor Parella

Magnetic Resonance in Chemistry 2017 (DOI: 10.1002/mrc.4695)

Abstract

A 1H-1H TOCSY experiment incorporating 13C multiplicity information is proposed. In addition, broadband 1H homodecoupling in the indirect dimension can be implemented using a perfect BIRD module that affords exclusive 1H chemical shift evolution with full decoupling of all heteronuclear and homonuclear (including 2JHH) coupling constants. As a complement to the normal TOCSY and the recent PSYCHE-TOCSY experiments, this novel multiplicity-edited TOCSY experiment distinguishes between CH/CH3 (phased up) and CH2 (phased down) cross-peaks which facilitates resonance analysis and assignment.