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Techniques & Tools Sample Preparation

Putting Sample Prep Centerstage

Sample preparation has achieved exceptional progress over the past few decades; we’ve seen the introduction of powerful technologies, advances in fundamental knowledge, and a plethora of breakthrough applications. However, enthusiasm for sample preparation is not necessarily shared by all members of the analytical chemistry community – let alone other scientific disciplines.

The idea that sample preparation is an “art” and not a “science” or that the discipline relies on application-driven research remains well-entrenched in the minds of many academics and non-academics. Indeed, sample preparation scientists have, on the whole, done a poor job of communicating contemporary advances and celebrating the successes of the field. There has been a lack of communication with external platforms, and an absence of credible and influential voices to articulate sample preparation’s importance and contributions.

Until very recently, internal communication within the sample preparation community has also been lacking. And a coherent strategy, outlining the goals, expectations, successes and future directions, did not exist. Moreover, a systems approach is rarely applied in sample preparation, meaning that it was often separated from the context in which it was conducted – and that its practice was not always considered in relation to its impact on many interconnected systems.

We believe the time is right for sample preparation to cast off its image as a “follower” discipline and take up its rightful place as a leader in discovery.

Using the force


In 2019, the European Chemical Society-Division of Analytical Chemistry (EuChemS-DAC), approved the formation of a new Task Force focusing on sample preparation with three objectives: i) to increase the visibility of sample preparation, ii) to raise awareness of its importance and contributions, and iii) to provide a coherent strategy for external and internal communication. To achieve these ambitious goals, the Sample Preparation Network was created as a space for academic and non-academic members of the sample preparation community to work collectively towards promoting, improving, and synchronizing activities.

Several European Committee Members were invited – and the participation of non-European experts was also encouraged to allow transparency and dissemination of the combined efforts. Today, the network includes regular members from 23 countries working in academia, institutes, industry, and private laboratories. Since its inception, three working groups have been created: “Science and Fundamentals,” “Automation, Innovation and Entrepreneurship,” and “Information Exchange and Networking.”

Minding the gap


We’ve seen a tremendous shift in the role of sample preparation from the early years of this century to the present. Initially, the focus was on determining trace-level concentrations of target contaminants in a large number of environmental or biological samples. Today, our efforts are more commonly directed toward more complex tasks, such as human exposomics – multidisciplinary and holistic approaches for untargeted and targeted workflows to uncover cancer biomarkers using mass spectrometry-based omics techniques. And also consider preliminary screening tests for rapid diagnosis at the bedside (so-called point-of-care analysis), which typically rely on affinity microextraction methods.

We will see the rise of post-pandemic efforts to improve robustness and independence – an important trend that must be reflected in analytical chemistry laboratories.

To achieve better results in these new areas, fabrication of new sorptive phases that improve selectivity towards class compounds or enhance sample clean-up in eliminating matrix interfering compounds is critical. To meet the need, there is a plethora of novel composite materials described in the literature and applied to complex samples; however, the majority do not perform better than commercially available materials – and validation across sufficient numbers of samples is rarely performed. Consequently, a gap has opened up between promising research results and sample preparation products that actually make it to the market. Efforts in our Task Force and Network are directed toward filling that gap by gearing research efforts in Europe and the rest of the world towards actual needs; for example, the reliable detection of COVID-19 virus at very low-level concentrations by exploiting bioaffinity sorptive platforms.

The COVID-19 pandemic teaches us that modern society is fragile, and supply chains are not as reliable as we may like to think. Therefore, we will see the rise of post-pandemic efforts to improve robustness and independence – an important trend that must be reflected in analytical chemistry laboratories. Society depends heavily on our measurements, and labs must be able to stay fully operational during future crises. One scenario is to downscale analytical methods, reducing our consumption of chemicals and reagents. Another scenario is to analyze samples on-site with smartphones, operated by non-trained personnel, and connected to a network for digital or manual interpretation. In a more pessimistic scenario, sampling and analysis may have to become contactless; for example, using drones for field sampling and automated laboratory methods with all sample preparation steps fully integrated. All these scenarios rely on extensive sample preparation research, and development of new micro-extraction technologies.

Braving a new world


Digital technology is already having a major impact on sample preparation. The breadth of materials and composites now available, each with distinct chemical composition and sorptive properties, opens new possibilities for 3D-printing tailor-designed sorbent materials, membranes and scaffolds for point-of-use devices. By the year 2040, analytical chemistry will likely be staffed with scientists born with a smartphone or tablet in their hands and a 3D printer at home. The thirst for data will unite them with wider societal forces, and members of the public will be actively engaged with “citizen science,” transforming analytical research. The rise of connectedness and low-cost sensor technologies used for chemical measurements, as well as the push to improve the transparency and accessibility of science, will require many enabling technologies, including advances in smartphone cameras and printer resolution; new (open source) software; detectors/detection principles compatible with the 3D-printed (open source) objects; smartphone compatible microchips; lab-on-paper; and, last but not least, sample preparation. The latter has to be microscale to adapt to the microchip format and highly selective to circumvent the limited selectivity of smartphone sensors.

Much of this future relies on extensive sample preparation research – and we must find new ways to reinvigorate the area by bringing in other disciplines, while still maintaining the field’s identity.
 

Global Impact

EuChemS-DAC Sample Preparation Task Force first launched in Europe, but soon expanded to include international members. Here, four international committee members from around the world share their hopes for the initiative.

Janusz Pawliszyn, University of Waterloo, Canada

The EuChemS-DAC Sample Prep Task Force and Network will engage committed individuals to move the analytical science towards a greener, more sustainable future. There are a number of new, efficient extraction technologies based on fundamental research, but the majority of scientists are either not aware of these developments or do not understand them.  When chemists get involved in a project involving a quantification step, they typically want to provide the necessary data ASAP. As such, familiar approaches are preferred, and newer, more powerful, and greener techniques are ignored in favor of standard technologies that may not fully address the challenge at hand. In an ideal world, scientists would consider the utility of all approaches when tackling a problem; however, this is rarely done in practice. This phenomenon is not limited to analytical chemistry or even chemistry but is observed whenever new technologies are introduced. However, we are living in times when swift and decisive action is needed towards a sustainable future. We have many technologies already available or under development that can support human existence on the Earth for millions of years to come, and we must make use of them if future generations are to enjoy life as we have experienced it.  The leadership provided by the Task Force towards cost-effective and faster screening methods will prove central to address these challenges.

Gangfeng Ouyang, Sun Yat-sen University, China

Sample preparation is a classical research field, which has exerted wide and deep impacts on our modern society. However, even as the importance of the field grows, there is waning interest from the scientific community; many scientists appear to be convinced that the fundamentals of sample preparation can be addressed by the classical theories and laws of thermodynamics and mass transfer, and treat it as a purely application-driven research field. The Sample Prep Task Force and Network will be an invaluable international effort to raise awareness of the importance of sample preparation, promote scientific research in this field, and solve the problems encountered by different industries. China arguably has the largest number of researchers in this field, and we have seen similar initiatives on a national level, with regular academic meetings. Nonetheless, the clear and ambitious goals proposed by the EuChemS-DAC will certainly inspire researchers in China to organize more effective communication among research groups and individuals, as well as between industry and academia.

Fernando M. Lanças, University of São Paulo at São Carlos, Brazil

Sample preparation has applications in almost all areas in which chemical determinations are required. Unfortunately, most sample prep developments have been reduced to an appendix within the analytical chemistry niche, scattered across a large number of scientific periodicals in distinct disciplines. The recently created Task Force aims to increase the visibility of the community and promote external and internal communication of technical advances. In the current international landscape, I can envisage two avenues along which the Task Force can develop. Firstly, by including in its main efforts top international scientists and young investigators from developed countries, the network can widen its potential coverage and practical results in the sample prep arena. Secondly, the network could work with underdeveloped countries through educational programs to promote the many gains obtained by changing from the classical sample prep methods to the new technologies that allow: i) higher overall analytical efficiency and throughput, ii) a lower cost per analysis, and iii) less exposure to toxic materials.

Jared L. Anderson, Iowa State University, USA

The development of a Sample Preparation Task Force is a great way to educate the broader community about the importance of sample preparation in many interdisciplinary fields of science, ranging from molecular biology to environmental analysis. A critical role for the Task Force is to publicize the fact that sample preparation is still undergoing rapid change and that many of the advancements are in response to demands and techniques developed by the broader scientific community. I believe the initiative will bring more attention to the field and help significantly in recruiting new generations of scientists. On the global scale, I think that the efforts by the Task Force will enable more collaborative opportunities – and this will most certainly spread to other areas of study in which sample preparation procedures are still considered a major bottleneck in the workflow. It is an exciting time to be working in the field of sample preparation and I am particularly excited to see the team’s efforts pay off!

Reaching for the stars


Sample preparation needs to become increasingly interdisciplinary, if we are to increase opportunities for innovation. The Sample Preparation Task Force and Network will increase interaction with other sciences and promote problem-driven research to address the world's increasingly complex and interconnected problems.

Breaking down the single-discipline silos of sample preparation will also allow transferal of knowledge from other “distant” disciplines and will increase current understanding of the underlying processes. Indeed, compared with other physicochemically simpler systems, such as GC, sample preparation is less developed and understood. Focusing on the science is not about giving academics the freedom to explore their intellectual curiosities – it is the bedrock for future advances. We simply do not understand the technologies we use well enough to predict everything we need or might need; studying the fundamentals will future-proof the field and allow us to tackle problems we can’t yet foresee.

By introducing better financial incentives, we can better explore the nexus of technology and society, and encourage collaboration with the private sector.

Sample preparation is a creative science in itself, which should be practiced in both fundamental and applied arenas for the benefit of society. The EuChemS-DAC Sample Prep Task Force and Network will highlight the context within which sample prep is conducted and guide research towards areas with the greatest potential impact. A systems thinking approach will embrace green analytical chemistry, so that we are able to move towards sustainable science and meet the challenges of multiple unfolding world issues.

Just as important, EuChemS-DAC Sample Prep Task Force and Network will strengthen the interface between academia and the private sector. It will serve as the meeting point for academics and non-academics, and a hub for the exchange of information. By triggering demand-driven research, we can transform knowledge generated in universities into economic, social, and/or environmental value, bridging the gap between research and the demands of stakeholders. The EuChemS-DAC Sample Prep Task Force and Network will also work on initiatives aiming to spread the culture of entrepreneurship between academics. By introducing better financial incentives, we can better explore the nexus of technology and society, and encourage collaboration with the private sector.

Last but not least, we will strongly promote the inclusion of early-stage researchers and early career investigators. Giving this younger generation a voice on sample preparation through active participation and networking will feed into successful future career development.

Getting involved


An open invitation for membership is extended to European and non-European professionals with an interest in sample preparation, including both senior and early-career scientists. Becoming a member is easy and free. All members of our network can increase their networking opportunities, gain visibility by sharing their work with other members, participate in our activities for dissemination of the relevance of sample preparation in many disciplines and get the latest updates in the area.

And that’s not all. The Sample Preparation Task Force and Network organizes special sessions focusing on Sample Preparation in Euroanalysis and other major International Conferences running in Europe. A sample preparation course is also organized on an annual basis and serves to provide hands-on training on a variety of methods; the course moves around Europe and takes focus on different topics within sample preparation with each host.

More details on the Sample Preparation Task Force and Network and information on how to become a member are available at www.sampleprep.tuc.gr. Join us to champion the importance of sample preparation across multiple arenas!

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About the Authors
Stig Pedersen-Bjergaard

School of Pharmacy, University of Oslo, Norway, and Department of Pharmacy, University of Copenhagen, Denmark.


Elia Psillakis

Head of the EuChemS-DAC Sample Preparation Task Force and Network, Technical University of Crete, Greece.


Manuel Miró

Core Member of the EuChemS-DAC Sample Preparation Task Force, University of the Balearic Islands, Spain.

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