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. 2022 Mar 30;14(2):549–551. doi: 10.1007/s12551-022-00946-6

Solid-state NMR and hyperpolarization methods for the Research, Development, and Innovation in Costa Rican science

Isaac F Céspedes-Camacho 1,✉, Jörg Matysik 2
PMCID: PMC9043162  PMID: 35528032

Abstract

Inter and multidisciplinary collaborations are essential to achieve significant improvements in science and technology. Nuclear Magnetic Resonance (NMR) is a versatile technique that permits connecting different scientific disciplines. Therefore, its implementation and extension in several research fields will help to improve Costa Rican Research and Development. This Commentary intends to present the importance of NMR for Costa Rican science, by numbering some solid-state NMR applications that could be useful and attainable for the country, and by highlighting the advances in the use of hyperpolarization methods.

Costa Rican research and development (R&D) expenditure is less than 0.4% of their gross domestic product (GDB) (The World Bank 2022), quite far from the average of the Organization for Economic Cooperation and Development (OECD) members—spending almost 2.6% of their GDP—or the European Union countries. Therefore, a broader scientific and technological perspective must be attained by a multi and interdisciplinary collaboration. Novel scientific disciplines have been introduced in the country during the last decade, thanks to a significant governmental investment, trying to diversify and specialize their academic staff. Nevertheless, stronger collaboration between those disciplines is essential if the country want to diversify their research aims.

Liquid-state nuclear magnetic resonance (NMR) has played a significant role in the development of Latin American science, especially as a characterization technique in structural elucidation, and Costa Rica has not been the exception. Since 1970, researchers at the University of Costa Rica (UCR) have been doing NMR work with the only two high-field NMR spectrometers in Central America, first a 400 MHz followed by the acquisition of a 600 MHz. Costa Rican chemists have used NMR as a tool to determine chemical structures, almost exclusively of organic samples, strongly focused on natural products (Calderón et al. 2014; Chavarria et al. 2008). Results have been fruitful, leading to some well-established research groups (García-Barrantes et al. 2013; Montoya-Arroyo et al. 2020). At this time, investigations on different research fields demand the use of liquid-state NMR applications. However, the use and development of solid-state NMR in the region has been quite slow and not so visible and recognized as solution-state NMR. One of the main reasons being the anisotropic interactions that broaden spectral lines and hinder the extraction of structural information. By removing (or averaging) those anisotropic interactions new solid-state NMR in varied scientific and technological fields become available.

Researchers could use solid-state NMR spectroscopy to study local structural environments by bonding information and dynamic structural changes (Ashbrook et al. 2018). Solid-state NMR can be complementary to X-ray diffraction studies—that are becoming increasingly popular and a useful tool in Costa Rican science—to get a more detailed picture of a sample. Research groups working on micro- and mesoporous materials, such as metal organic frameworks or zeolites, can add solid-state NMR studies to get a comprehensive picture of the chemical and electronic structure of those materials.

Although options have been developed to overcome the issue, resolution continues to be a major problem in solid-state NMR. Magic-angle spinning (MAS) is a technique in which fast rotation of the sample around a fixed angle, increases the NMR resolution, especially for I = ½ nuclei (Levitt 2008).

The applications of MAS NMR spectroscopy are quite numerous. For example, it can be used in metabolomics—an active research field in Costa Rican labs—by getting the metabolic profile of plants, without requiring the extraction of the metabolites from the sample (Augustijn et al. 2021). Introduction of this application would save time and other resources. In a tropical country, where researchers study exotic plants, a combination of multivariate analysis and MAS NMR provide new and innovative strategies to study plant metabolomics.

Advances in NMR instrumentation, improvements in automation and the development of user-friendly software, invite other scientific disciplines in Costa Rica to start considering solid-state NMR spectroscopy. For example:

  • i.

    Food Science. Academic institutions, governmental labs, and the food industry can obtain detailed and useful information from food matrices. This approach is particularly suitable for countries like Costa Rica, where the economy depends significantly on the primary sector. Analysis of biopolymers in granular state and as food components, carbohydrate composition, components of cell walls and fibers in foodstuff, or even the metabolome of fruits and vegetables are all possible with solid-state NMR (Janovick et al. 2020).

  • ii.

    Cultural heritage. Simple solid-state NMR pulse-sequences allows the analysis of organic and inorganic components in historical and archeological artifacts made of materials such as rubber, wood, textiles, or paper (Lambert et al. 2016). Costa Rican archeologists, chemists, and even historians could gain a general overview of the structure of artifacts and draw useful information pertaining to historical material treatments, human behavior, or possible conservation protocols.

  • iii.

    Protein structure. Dynamically disordered or heterogeneous systems are especially suited to solid-state NMR studies. It is possible to elucidate the structure and dynamics of many membrane proteins (by the chemical shifts on multidimensional NMR), and to characterize amyloid proteins or other protein complexes (Reif et al. 2021). Biology, microbiology, and biotechnology research centers in Costa Rica could benefit from such uses of solid-state NMR spectroscopy.

Several methods—normally called hyperpolarization—have been developed to overcome the intrinsically low sensitivity of the NMR technique, leading to significant enhancements, in both liquid and solid state (Kuhn 2013). Some of the most useful hyperpolarization methods are dynamic nuclear polarization (DNP), chemically induced dynamic nuclear polarization (CIDNP), parahydrogen-induced polarization (PHIP), and hyperpolarized (HP) 129Xe. These methods are applicable in current Costa Rican research areas, such as porous materials and large biomolecular complexes. Although these methods tend to be expensive and are relatively unknown to NMR Costa Rican users, improvements have been made over the last years, especially on the spectroscopic characterization of zeolites and aerogels.

Integration of solid-state NMR and hyperpolarization in Costa Rica should start in the academia, by integrating these topics in the curricula of students majoring in Chemistry, Material Science Engineering, Biotechnology, Biology and Physics. Since 2018, the Chemistry MS program at the UCR offers a course that is unique on its kind in Latin America: Solid-state NMR and hyperpolarization methods. Enrollment is open to national and international students, and students from disciplines other than Chemistry. After taking this course, some students have implemented hyperpolarization methods on their final projects and theses. For example, an Environmental Engineering major used the solid-state photo-CIDNP effect to study the spin chemistry on photosynthetic organisms and its potential use as an energy source (Vega-Cárdenas 2020). Two students—one Chemistry major, the other Material Science Engineering major—used HP 129Xe to study the structure of some inorganic adsorbents in a novel fashion (Barboza-Carmona et al. 2022; Puente-Urbina et al. 2016). Additionally, NMR work has been presented in some of the most important NMR meetings, such as Euromar or the GDCh FGMR Annual Discussion Meeting, and has been part of keynote lectures in some national conferences, such as the Costa Rican Biophysics Symposium or at the Costa Rica National Academy of Sciences (Solís et al 2021). Also, Costa Rican students have received grants to participate in summer schools on theory on NMR organized by one of the authors in Leipzig, Germany. These events provided advanced NMR theoretical training. Likewise, solid-state NMR short courses have been organized in Costa Rica, with the participation of NMR researchers from Europe and the USA.

Students will have to learn about the solid-state NMR theory and applications—including the hyperpolarization methods—to expand the horizon of possibilities in their fields. In the current globalized world, Costa Rican science must diversify by learning new approaches and apply them in innovative, attractive, and inclusive ways. The size and cost of instrumentation for solid-state NMR is a major drawback for its application in Costa Rica national industry and academia. Nevertheless, significant progress in the field can be achieved with the development of smaller, cheaper, more robust, and portable benchtop NMRs.

Declarations

Ethical approval

This article does not contain any studies with human participants or animals performed by the authors.

Consent to participate

Not applicable

Consent to publish

Not applicable

Competing interests

The authors declare no competing interests.

Footnotes

Publisher's note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

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