Category Archives: NMR Events & Courses

News about courses, workshops, seminars, conferences and any other training activity related to the SeRMN.

SeRMN contribution at SMASH 2019

Kumar Motiram-Corral presented a poster titled “Implementing one-shot multiple-FID acquisition into homonuclear and heteronuclear NMR experiments” at SMASH 19 in Porto (Portugal).

To date, time-efficient approaches are a challenged task for spectroscopists.  The goal is to obtain chemical information reducing experimental time without considerably losing of sensitivity.

Different time-efficient approaches have been described over the years.  Time sharing (Parella et. al.) tactic acquires the 15N and 13C nuclei in the same spectrum in spectrometers which have a triple channel hardware configuration[1].  Non-Uniform Sampling (NUS) [2] algorithm has achieved a substantial reduction of experimental time reducing the number of t1 increments needed by multidimensional experiments.  Recently, NOAH [3] (NMR by ordered Acquisition using 1H detection) has been developed by Kupče (Bruker Co.) and Claridge (University of Oxford) provides the way to get proper experiments in different spectra with the same spectral quality.

[4]MFA (Multiple FID Acquisition) consists in obtaining up to four different experiments decreasing close to 60% of time.  MFA provides a new novel proof concept of COSY, TOCSY and HMBC experiments in small molecules.  Actually, MFA strategy was proposed many years ago with the COCONOSY experiment [5-7],  which could be collected 2D COSY and NOESY data with a single pulse scheme.  [4]MFA has also been implemented in magic-angle-spinning solid-state NMR experiments devoted for biomacromolecules using standard spectrometer configuration.  Despite its limitations related to the use of long acquisition of free-induction decays (FIDs) to accurately digitalize the data and the mandatory use of long phase cycles for convenient pathway selection, nowadays, the use of pulsed field gradients (PFGs) is the solution for this drawback.  [4]MFA is based on the relaxation of the remaining transverse magnetization, which usually relaxes to its original magnetization, can be manipulated by an appropriate additional mixing process and recorded again to obtain a second or third NMR data provided that T2 (transverse relaxation times) are long enough.  [4]Its main advantage is that each experiment is acquired in a different display.  [4]MFA is a powerful experiment for the sequential structural assignment of a whole spin system without ambiguities.  This method is also useful for selective experiments as SE-TOCSY.

References: 

  1. Nolis, P., Pérez, M., & Parella, T. (2006). Time-sharing evolution and sensitivity enhancements in 2D HSQC-TOCSY and HSQMBC experiments. Magnetic Resonance in Chemistry, 44, 11, 1031-1036, 2006
  2. K. Kazimierczuk and V. Y. Orekhov , Angew. Chem., Int. Ed., 2011, 50 , 5556 -5559
  3. Kupče, E., & Claridge, T. D. W. (2018). Molecular structure from a single NMR supersequence. Chemical Communications, 54, 7139-7142, 2018.
  4. Motiram-Corral, K., Pérez-Trujillo, M., Nolis, P., & Parella, T. (2018). Implementing one-shot multiple-FID acquisition into homonuclear and heteronuclear NMR experiments. Chemical Communications, 54(96), 13507–13510, 2018.
  5. A. Z. Gurevich , I. L. Barsukov , A. S. Arseniev and V. F. Bystrov , J. Magn. Reson., 56, 471 -478, 1984. 
  6. C. A. G. Haasnoot , F. J. M. van de Ven and C. W. Hilbers , J. Magn. Reson.56 , 343 -349, 1984. 
  7. J. Cavanagh and M. Rance , J. Magn. Reson., 14 , 408 -414, 1990. 

SeRMN contributions at ISMAR EUROMAR 2019 Conference

Some of the SeRMN staff will present our last research works at the annual meeting of the European magnetic resonance community ISMAR EUROMAR 2019 Conference that will take place from 25th to 30th August in Berlin. Find below a summary of our contributions.

Pau Nolis presents a poster entitled “Reducing experimental time using Multiple Fid Acquisition (MFA) strategy” (P341). Pau Nolis, Kumar Motiram-Corral, Miriam Pérez-Trujillo, Teodor Parella.

Speeding-up NMR molecular analysis is an important research field which has been continuously advancing since NMR early days. The relevant benefits are clear and evident: reduce the time per analysis directly reduce its cost and gaining spectrometer time to analyze new samples. Many interesting tools and concepts have been appearing in last decades. Concretely, our experience focuses on the development of new NMR experiments using TS (Time-Shared), SA (Spectral Aliasing) and MFA (Multiple Fid Acquisition). MFA strategy is an interesting strategy that allows the acquisition of different structural information in a single experiment. Basically, MFA experiments consist in the design of pulse sequence experiments which accommodate several acquisition windows per experi-ment, each registering different relevant information for the structural molecular character-ization. The methodology brings a corresponding important time benefit. Last year, we have reported several new NMR experiments designed with MFA stratey and herein we would present the most relevant achievements. The overall discussion will be mainly focused on the sensitivity gains per time unit of the presented experiments.

Eva Monteagudo presents a poster entitled “Enantiodifferentiation Study of Spiroglycol Chirality” (P306). Eva Monteagudo, Albert Virgili, Teodor Parella, Carles Jaime.

The 3,9-bis(1,1-dimethyl-2-hydroxyethyl)-2,4,8,10-tetraoxaspiro[5.5]undecane commonly named pentaspiroglycol (PSG) or spiroglycol (SPG) is a high molecular weight rigid alicy-clic diol widely used in the chemical industry. SPG has no hazardous classification, it is not mutagenic and is a safe alternative to Bisphenol A, a well-known chemical which is rising concern due to his proved endocrine disruptor activity. Moreover, some of the SPG main applications are focused on epoxy resins, liquid polyester resins, radiation curing resins and in polymer film material field. However, the spiroglycol structure, configuration and conformation have never been deeply studied. Herein, we perform for the first time a preliminary NMR and computational study of the spiroglycol structure. SPG is a highly symmetrical molecule but it should be chiral due to the presence of a chiral axis. The presence of two enantiomers was demonstrated per-forming NMR enantiodifferentiation experiments using α,α’-bis(trifluoromethyl)-9,10-an-thracenedimethanol (ABTE) as chiral solvating agent (CSA). The addition of 0.6 equivalents of ABTE allows the differentiation of several spiroglycol proton signals. The lack of resolu-tion observed in the proton spectrum can be tackled through the corresponding 13C NMR spectrum where a significant enantiodifferentiation at the spirocarbon atom was observed.In order to physically separate both enantiomers, a SPG derivatization with camphor-sulphonic acid was performed affording the corresponding diastereoisomeric ester mixture.

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 ()

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.

SeRMN contribution to Symmetry 2017 Conference

 

Some of the SeRMN staff  presented our last research work about chirality at The first International Conference on Symmetry, Symmetry 2017, that took place from16th to 18th October in Barcelona. Find below a summary of our contribution.

Míriam Pérez-Trujillo presented a lecture entitled: “Chiral Recognition by Dissolution Dynamic Nuclear Polarization NMR Spectroscopy

Abstract: The recognition of enantiomeric molecules by chemical analytical techniques is still a challenge. A method based on d-DNP (dissolution dynamic nuclear polarization) NMR spectroscopy to study chiral recognition was described for the first time [1]. DNP allows boosting NMR sensitivity by several orders of magnitude, overcoming one of the main limitations of NMR spectroscopy [2]. A method integrating d-DNP and 13C NMR-aided enantiodifferentiation using chiral solvating agents (CSA) was developed, in which only the chiral analyte was hyperpolarized and selectively observed by NMR. The described method enhances the sensitivity of the conventional NMR-based procedure [3] and lightens the common problem of signal overlapping between analyte and CSA. As proof on concept, racemic metabolite 13C-labeled DL-methionine was enantiodifferentiated by a single-scan 13C NMR experiment. This method entails a step forward in the chiral recognition of small molecules by NMR spectroscopy; it opens new possibilities in situations where the sensitivity is limited, for example, when low analyte concentration available or when measurement of an insensitive nucleus required. The advantages and current limitations of the method, as well as future perspectives, are discussed.

Presentació Software RMN Mnova (Mestrelab)

Esteu convidats a la presentació del software Mnova (Mestrelab Research) el proper dimecres 1 de Març a l’aula C1/009, de 15:30 a 17:30. És una eina de gran utilitat per qualsevol químic interessat en el processament/manipulació rutinàri/a de  dades de RMN (i altres tècniques analítiques) d’una manera ràpida, eficient i molt intuitiva. Es presentarà les novetats més importants de la nova versió Mnova11 així com es resoldrà qualsevol qüestió pràctica que es plantegi.

You are invited to the presentation of the new Mnova software package (Mestrelab Research) on Wednesday March 1st in class C1 /009, from 15:30 to 17:30. It is a useful tool for any chemist interested in processing / handling routine NMR data (and other analytical techniques) in an efficient and intuitive way. The most important developments of the new version Mnova11 will be presented and practical question of interest will be discussed.

10th Workshop on Magnetic Resonance Spectroscopy and Imaging (MRI/MRS) Applied to Laboratory Animals

Workshop dates: November 29th – December 2nd, 2016
Registration deadline: November 14th, 2016
Registration: REGISTRATION CLOSED  online
Capacity: Workshop limited to 4 participants (first come, first served)
Contact person: Silvia Lope-Piedrafita, PhD ()

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.20161001_10cursomrimrs

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

SeRMN at the SMASH NMR 2016 Conference

Some of our last research works has been presented at the annual meeting of the SmallMolecule NMR Conference (SMASH) that has been taken place in La Jolla (USA) from 11thto 14thSeptember 2016.

Teodor Parella presented two posters.
“In situ determination of 1DCH and 2DHH RDCs from a single 1JCH/2JHH -resolved NMR measurement” of Núria Marcó García, Roberto R. Gil and Teodor Parella.

Abstract: A fast RDC-assisted strategy involving the simultaneous determination of isotropic (scalar) and anisotropic (total) interactions is reported. The concerted use of individual 1DCH for all CHn multiplicities and 2DHH obtained from a single 1JCH/2JHH-resolved NMR spectrum offers an unambiguous assignment of diastereotopic protons and an efficient discrimination between all eight possible diastereoisomeric structures of strychnine which contains six stereocenters.

Figure: 500.13MHz JCH/JHH-Resolved spectra of 1 in A) isotropic CDCl3 and B) anisotropic PMMA-CDCl3 (2H nQ(CDCl3)=26 Hz) conditions. The projections along the F2 dimension are the conventional 1H spectrum in isotropic conditions and the 1H-CPMG spectrum in anisotropic conditions, respectively.

“Pure shift NMR covariance” of André Fredi, Pau Nolis, Carlos Cobas, Gary E. Martin, Teodor Parella.

Abstract: The development of novel experimental strategies to significantly enhance signal resolution by broadband homodecoupling is a current topic of high interest in 1H NMR spectroscopy . A number of different building blocks have been implemented into 1D and 2D homo- and heteronuclear experiments in order to provide resolution-enhanced pure chemical shift 1H NMR spectra, where signals appear collapsed to singlets. On the other hand, Covariance processing methods have been used to generate challenging NMR spectral representations . We present here the first attempts towards a general solution to generate Pure Shift NMR spectra by using Generalized Indirect Covariance (psGIC) co-processing3,4 . The current strategy is based on the calculation of a new 2D psGIC spectrum from the combination of a parent homo- or heteronuclear spectrum and a reference 2D F1-homodecoupled 1H- 1H correlation spectrum only showing diagonal cross-peaks (DIAG), which share a common 1H frequency dimension. Using psGIC, the F1 dimension in the DIAG spectrum is transferred to the F2 dimension of the parent spectrum, thus generating a new pure shift 2D spectrum

Figure: Generation of Pure Shift NMR spectra by using Generalized Indirect Covariance (psGIC)

André Fredi’s oral presentation at 8th GERMN / 5th Iberian NMR Meeting

André Fredi made an oral presentation at the 8th GERMN / 5th Iberian NMR Meeting (GERMN 2016) held in Valencia, Spain from 27th to 29th June 2016.

In his presentation, that was titled  Exploring the use of Generalized Indirect Covariance to reconstruct Pure Shift NMR spectra: Current Pros and Cons”, André explained how to make pure spectra shift from Generalized Indirect IMG-20160628-WA0028Covariance processing (psGIC). This new method is basically a new way to get “synthetic” pure shift spectra without the need to purchase a pure shift spectrum in the spectrometer and without the penalties that pure-shift experiments cause.

André has been working as a Ph.D. candidate at the Department of Chemistry and SeRMN under the direction of Dr. Teodor Parella and Dr. Pau Nolis since November 2014, when he enrolled in the Department of Chemistry doctoral program at Universitat Autònoma de Barcelona with a fellowship from CNPq-Brazil. He is currently in his second year and expects to defend the doctoral thesis on 2017/2018.

 

Presentations at the EUROMAR 2016 Conference

euromar

André Fredi (PhD student) and Teodor Parella presented our last research works at the annual meeting of the European magnetic resonance community EUROMAR 2016 Conference that was celebrated on days 3th to 7th July in Aarhus, Denmark. Find below a summary of our contributions. Continue reading Presentations at the EUROMAR 2016 Conference