 PFAS Are Everywhere — And 99% Go Undetected

<div><p><strong>Sample preparation is a critical step in the analytical process, transforming raw samples into analysis-ready materials that significantly impact downstream applications. Mastering sample preparation is essential for producing high-quality, reliable data across various fields, such as environmental monitoring, pharmaceutical development, food safety testing, forensic analysis, and research.</strong></p><p>Proper preparation ensures that samples accurately represent the substance being analyzed, free from contamination or background interferences. Consistent sample preparation methods enable reproducibility, allowing experiments to be reliably replicated by different labs or on different days. Sample preparation also enhances sensitivity, because detecting trace substances is crucial across forensic, clinical research, pharmaceutical testing and more. Streamlining the preparation process reduces time and resources, making analysis more efficient and cost-effective.</p><p>This article provides an in-depth exploration of sample preparation techniques, covering their principles, applications, and best practices to facilitate informed decision-making and optimal analytical outcomes.</p></div><div><div><div><div><h3><strong>Types of Sample Preparation Techniques</strong></h3><p>Sample preparation techniques can be categorized into several types based on the sample state and analytical requirements.</p></div></div></div></div><div><div><div><div><h3><strong>Solid Sample Preparation Techniques</strong></h3></div></div></div></div><div><p><strong>Homogenization and Grinding:</strong> Homogenization and grinding involve breaking down large particles into a uniform mixture to ensure representative sampling, using methods such as mechanical grinding with ball mills or mortar and pestle, cryogenic grinding with liquid nitrogen, or ultrasonic homogenization.</p><ul><li><strong>Drying:</strong> Drying removes moisture from samples to prevent interference with analysis, through methods including oven drying, freeze-drying, vacuum drying, and spray drying.</li><li><strong>Solid-Phase Extraction (SPE):</strong> The <a target="_blank" rel="noopener noreferrer" href="https://labrulez.com/en-us/all/products?category=136&amp;manufacturerItems=50"><strong>solid-phase extraction</strong></a> technique selectively retains analytes by retaining target analytes using solid sorbents, including reversed-phase sorbents like C18, normal-phase sorbents like silica, and ion-exchange sorbents like quaternary amine. A weak wash can be utilized to remove weakly bound sample impurities before a strong wash solvent releases the analytes for further analysis.</li><li><strong>Solid-Phase Microextraction (SPME):</strong> SPME is a solvent-free extraction technique that uses fiber-based or in-tube SPME to extract analytes from samples.</li><li><strong>Protein Precipitation:</strong> A technique in clinical research labs, proteomics or drug discovery labs to separate proteins from a solution or complex mixture. The process involves loading sample onto a media, mixing or centrifugation and vacuum extraction to remove the sample protein free. This can also be done in a tube with solvents but requires more centrifugation and precision in pipetting. Additionally, protein precipitation plus phospholipid removal products allow for simultaneous removal of proteins and phospholipids for improved MS results.</li></ul></div><div><div><div><div><h3><strong>Liquid Sample Preparation Techniques</strong></h3></div></div></div></div><div><p><strong>Dilution and Filtration:</strong> Dilution and filtration involve reducing analyte concentration and removing particulate matter from liquid samples using membrane filtration, glass fiber filtration, or centrifugation.</p><ul><li><strong>Liquid-Liquid Extraction (LLE):</strong> LLE separates compounds based on solubility in two immiscible liquids, using techniques such as separatory funnel extraction or continuous liquid-liquid extraction.</li><li><strong>Supported/Solid Liquid Extraction (SLE) or called Liquid-Solid Extraction:</strong> Liquid-solid extraction transfers analytes from liquid to solid phase using solid-phase extraction or liquid-solid chromatography.</li><li><strong>Dialysis:</strong> Dialysis separates molecules based on size through diffusion across semi-permeable membranes.</li></ul></div><div><div><div><div><h3><strong>Other Sample Preparation Techniques</strong></h3></div></div></div></div><div><p><strong>QuEChERS:</strong> <a target="_blank" rel="noopener noreferrer" href="https://www.phenomenex.com/techniques/quechers"><strong>QuEChERS</strong></a><strong> </strong>(Quick, Easy, Cheap, Effective, Rugged, and Safe) is a sample preparation technique commonly used in analytical chemistry for food and environmental analyses. QuEChERS is favored for its simplicity, speed, and cost-effectiveness, making it ideal for high-throughput laboratories analyzing complex matrices like fruits, vegetables, and other food products.</p><ul><li><strong>Microwave-Assisted Extraction:</strong> Microwave-Assisted Extraction (MAE) uses microwave energy to heat the solvent and sample, causing rapid thermal effects that enhance the extraction of target compounds. The microwave radiation penetrates the sample, leading to the vibration of polar molecules, which generates heat. This heating process disrupts the cell walls of plant or biological material, allowing faster and more efficient release of analytes into the solvent.</li><li><strong>Ultrasonic-Assisted Extraction:</strong> Ultrasonic-Assisted Extraction (UAE) employs high-frequency sound waves (ultrasound) to disrupt the cell structure of the sample material. Ultrasound causes cavitation (the formation of microbubbles) in the liquid, which collapses violently, generating localized high pressure and temperature. This leads to the breakdown of the sample matrix, enhancing mass transfer between the solvent and analyte.</li><li><strong>Supercritical Fluid Extraction:</strong> Supercritical Fluid Extraction (SFE) involves using fluid at its supercritical state (above its critical temperature and pressure) to extract analytes. In this state, the fluid exhibits properties of both a gas and a liquid, allowing it to diffuse like a gas and dissolve substances like a liquid.</li><li><strong>Pressurized Liquid Extraction:</strong> Pressurized Liquid Extraction (PLE), also known as accelerated solvent extraction (ASE), uses solvents at elevated and high pressures to extract analytes from solid or semi-solid matrices. Under these conditions, the solvent's viscosity and surface tension are reduced, improving its ability to penetrate the sample matrix and dissolve the analytes more efficiently.</li><li><strong>Immunocapture:</strong> A technique that uses antibodies to selectively isolate and concentrate specific target molecules, such as proteins, from a complex mixture. This method leverages the high specificity of antibodies for their antigens (target molecules) to achieve purification and enrichment of the target, which can then be analyzed or further processed.</li></ul></div><div><div><div><div><h3><strong>Optimizing and Implementing Sample Preparation Techniques</strong></h3></div></div></div></div><div><p>Validating and optimizing sample preparation methods is crucial to ensure accuracy, precision, and reliability. This involves evaluating several parameters, including recovery, precision, accuracy, robustness, and selectivity. Method validation protocols typically involve verifying the method's performance characteristics, such as detection limits, quantitation limits, and linearity.</p><p>Optimization techniques, such as experimental design and response surface methodology, help refine the sample preparation process. These approaches enable analysts to systematically evaluate the effects of various factors, including extraction solvent, temperature, and time, on the method's performance.</p><p>Even with validated and optimized methods, several issues may arise during <a target="_blank" rel="noopener noreferrer" href="https://www.phenomenex.com/techniques/sample-preparation"><strong>sample preparation</strong></a>.</p><ul><li>Contamination can occur through improper handling, storage, or equipment cleaning, leading to inaccurate results.</li><li>Analyte loss, low recovery, or degradation can result from inadequate stabilization, storage, or handling procedures.</li><li>Inconsistent results may stem from variations in the sample matrix, instrumentation, wrong solvent/phase selection, or operator technique.</li><li>Instrument malfunctions can compromise results.</li></ul><p>To address the common challenges in sample preparation, laboratories should identify root causes and apply corrective measures, such as re-examining sample handling and storage procedures, verifying instrument calibration, or adjusting method parameters. Additionally, following best practices and safety considerations is crucial to prevent accidents and ensure a safe working environment. This includes wearing personal protective equipment (PPE) and adhering to laboratory safety protocols for waste disposal and chemical handling.</p><p>Regular quality control measures are also vital to ensure reliable results. Laboratories should implement standard operating procedures (SOPs), verify reagent purity and stability, monitor environmental conditions, and maintain instruments through regular calibration and maintenance. Furthermore, continuous training and competency assessment for laboratory personnel are essential.</p><p>Implementation of these measures is crucial for laboratories to ensure the quality and reliability of their sample preparation methods, ultimately supporting accurate and meaningful analytical results.</p></div><div><div><div><div><h3><strong>Conclusion</strong></h3></div></div></div></div><div><p>Robust sample preparation has proven instrumental in fields like environmental monitoring (e.g., detecting isolating pollutants using SPE), pharmaceutical development (e.g., bioanalytical testing with LLE and SPME), and food safety clean-up (e.g., QuEChERS for pesticide residue analysis).</p><p>As analytical chemistry evolves, emerging trends like automation, miniaturization, and green chemistry will further enhance efficiency, sensitivity, and sustainability for sample preparation techniques. Ultimately, high-quality sample preparation is essential for delivering accurate, reliable, and groundbreaking research outcomes.</p></div>

Sample Preparation Techniques for Precision in Analysis

<p><strong>Seven shared laboratories at CEITEC Masaryk University have received LEAF certification, which helps research facilities reduce their environmental impact and use resources more efficiently. The certification marks a first step towards systematically introducing sustainable practices into laboratory operations and forms part of Masaryk University’s broader efforts to make its operations more sustainable.</strong></p><p>Scientific laboratories are energy- and resource-intensive workplaces. Their operation requires specialised equipment, chemicals, disposable supplies and facilities for the long-term storage of biological samples. Reducing their environmental impact, however, goes far beyond sorting waste or switching off instruments when they are not in use. Efficient use of equipment and materials, sharing resources and well-designed working procedures are equally important.</p><p>These are precisely the areas addressed by<strong> LEAF</strong> (<strong>Laboratory Efficiency Assessment Framework</strong>), an international certification programme developed by <strong>University College London</strong>. LEAF helps research facilities introduce sustainable laboratory practices and continuously assess how they operate.</p><p><strong>Seven shared laboratories at CEITEC MUNI </strong>have now achieved <strong>Bronze-level certification</strong>: Biomolecular Interactions and Crystallization (BIC), the Josef Dadok National NMR Centre (NMR), Proteomics, Cryo-Electron Microscopy and Tomography (CryoEM), the Multimodal and Functional Imaging Laboratory (MAFIL), Cellular Imaging (CELLIM) and Nanobiotechnology (Nanobio).</p><h3><strong>From sustainability strategy to everyday practice</strong></h3><p>Participation in the LEAF programme builds on the<strong> CEITEC MUNI Sustainability Strategy 2026–2028</strong>, which in turn follows Masaryk University’s university-wide sustainability strategy. The aim is to make sustainability part of everyday laboratory operations and establish a system for their continuous assessment and improvement.</p><p>CEITEC MUNI focused on its core facilities – shared laboratories that provide researchers with access to specialised technologies and expertise. Their equipment is used by researchers from different research groups and institutions, making efficient operation, resource sharing and consistent working procedures particularly important.</p><p><i>“We wanted to give our laboratories practical guidance on how to integrate sustainability into their everyday operations. It is not only about energy consumption or waste management, but also about the efficient use of equipment and materials, user training, the working environment and how teams function. LEAF has given us a framework that helps us improve these areas systematically,” </i>explains <a target="_blank" rel="noopener noreferrer" href="https://www.ceitec.eu/katerina-hoskova/u94418"><strong>Kateřina Hošková</strong></a>, Secretary for Research Infrastructures at CEITEC MUNI. <i>“Sharing equipment and infrastructure is also a very important principle from a sustainability perspective. I am therefore very pleased that the University is currently implementing a university-wide booking system for specialised equipment and services, which will make sharing more efficient,”</i> she adds.</p><p>One of the measures introduced as part of the LEAF certification was the appointment of <strong>sustainability ambassadors </strong>at individual facilities. They coordinate activities aimed at reducing the environmental footprint of their laboratories and bring sustainability topics into regular team meetings and day-to-day operations. A more systematic approach to sustainability has also influenced decisions about the purchase and operation of laboratory equipment.</p><h3><strong>Certification verifies how laboratories actually operate</strong></h3><p>LEAF offers three levels of certification – <strong>Bronze</strong>, <strong>Silver </strong>and <strong>Gold</strong>. Each includes requirements covering different aspects of sustainable laboratory operations.</p><p>Certification is not merely an administrative exercise. Facilities must demonstrate how they meet individual requirements. A subsequent audit verifies whether the submitted evidence reflects actual practice, including, where necessary, through an on-site visit to the laboratory.</p><p>The assessment also takes into account the specific conditions of individual facilities, which differ in their technologies, equipment and type of research. If a particular requirement is objectively not applicable to a laboratory, it may be marked as not relevant, provided this is justified. However, the number of criteria that can be excluded in this way is limited.</p><p>The programme also supports continuous improvement. Laboratories can assess their operations, identify areas for further development and gradually introduce more demanding measures, allowing them to progress to higher levels of certification.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Archiv_CEITEC_MU_laboratore_CEITEC_504d5708b9.jpg" alt="CEITEC MU:  More Sustainable Science Starts in the Lab" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Archiv_CEITEC_MU_laboratore_CEITEC_504d5708b9.jpg 234w," sizes="100vw" width="870" height="580"></p><h3><strong>Learning from international experience</strong></h3><p>When introducing the certification, CEITEC MUNI also drew on the experience of other European research institutions. Through its membership in the EU-LIFE alliance and involvement in its sustainability task force, CEITEC gained practical recommendations from the UK’s <strong>Francis Crick Institute</strong>, which has extensive experience with the LEAF framework.</p><p>“The experience of our colleagues at the Francis Crick Institute helped us understand how to implement the certification in practice and how to assess the individual criteria. International cooperation allowed us to build on approaches that had already been tested at another major research institution,” adds Kateřina Hošková.</p><h3><strong>A concrete contribution to Masaryk University’s sustainability strategy</strong></h3><p>By achieving LEAF certification, CEITEC MUNI is contributing to Masaryk University’s university-wide sustainability strategy, which includes responsible resource management and the integration of sustainable development principles into the University’s operations.</p><p><i>“Sustainability is an important topic for Masaryk University, and we are gradually integrating it into all areas of how the University operates. CEITEC demonstrates that even in the highly specialised environment of scientific laboratories, there are practical ways to use resources more responsibly. We greatly appreciate initiatives from our colleagues that help turn the University’s sustainability strategy into practice,”</i> says <strong>Blanka Machová </strong>from<strong> Masaryk University’s Sustainability Office</strong>.</p><p>The experience of the participating core facilities can also inspire other research facilities at Masaryk University to make their laboratory operations more sustainable.</p><p><i>“CEITEC has long demonstrated that it can be a pioneer not only in science, but also in introducing new approaches to how research facilities operate. LEAF certification is another tangible result of these efforts. We are pleased to see initiatives emerging at Masaryk University that can serve as an example to others. We believe that CEITEC’s experience will help support more sustainable laboratory operations at other parts of the University as well,” </i>says <strong>Richard Hubl</strong>, <strong>Director of Masaryk University’s Administrative and Operational Support Department</strong>.</p><p>Achieving Bronze certification is not the end of the process. CEITEC MUNI plans to recertify its laboratories annually and introduce further measures that may enable some facilities to reach higher levels of certification in the future. The aim is for sustainability to become a natural part of their day-to-day operations and to deliver lasting results.</p>

 More Sustainable Science Starts in the Lab: Seven CEITEC MUNI Facilities Receive International Certification 

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