Hexane, a health and regulatory risk for food and non-food products:
Its elimination from analytical protocols can improve consumer protection

Laurence JACQUES - EcoXtract / France

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Hexane, a health and regulatory risk for food and non-food products: why eliminating hexane from analytical protocols can improve consumer protection.

Hexane, a neurotoxic petroleum oil, suspected of being a reprotoxic and endocrine disruptor, is still widely used today to extract edible oils and natural extracts. Hexane extraction is, in fact, very efficient and cost-effective. However, its use contaminates extracted products and the products of animals fed with extracted products. Oils, flavors, fragrances, proteins or defatted cocoa, eggs, butter, cosmetic ingredients, and nutraceutical products are found to be loaded with residues. EFSA, the European Food Safety Authority, published a report in September 2024, recognizing that public protection was not guaranteed and that the food authorization of hexane should be reviewed. This review began in May 2025 and its conclusions are expected by November 2027.

Furthermore, in February 2025, hexane was added to the list of Substances of Very High Concern, the European blacklist of chemicals. Substances on this list are expected to be banned in Europe within a few years. Finally, in March 2025, MODEM MP Richard Ramos tabled a bill in the National Assembly to require the traceability of hexane and then its gradual elimination.

It was the detection of hexane residues in everyday products that contributed to the mobilization of politicians and civil society actors. What are the measurable levels of hexane residues in food and non-food products? Hexane is still used today for many laboratory protocols. The ubiquity of this pollutant in many analytical platforms is an obstacle, in some cases, to the development of methods with better detection limits. This difficulty, coupled with hexane's inclusion on the list of substances of very high concern, the chemical blacklist, raises the question of hexane's substitution in laboratory protocols. What alternatives to hexane are currently available? How can we move towards greener analytical methods?

Coming of age of multidimensional liquid chromatography.
Bridging the gap between research and modern analytical workflow.

Gerd Vanhoenacker, Research Institute for Chromatography, RIC Group, Belgium

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Multidimensional chromatography is extremely powerful for the comprehensive analysis of complex samples, offering significantly enhanced peak capacity that allows for the resolution and quantification of analytes otherwise obscured by the matrix.

While two-dimensional gas chromatography (2D-GC) has matured and found its way into various workflows and industries, the implementation of two-dimensional liquid chromatography (2D-LC) in routine analytical laboratories has historically been hampered by challenges in method development, hardware configuration, and data processing.

Recent and targeted advances in 2D-LC hardware and software significantly reduce the complexity barrier for non-expert users allowing the technique to be applied outside of the academic and pure research environment.

The presented findings confirm the operational maturity of modern 2D-LC for integration into day-to-day analytical workflows, prompting discussion on its imminent role as a standard tool in state-of-the-art analysis.

Capillary electrophoresis: beyond R&D, towards high-volume analysis
with negligible chemical consumption or waste

Noah WEISS - Customer Analytical Services Lab (CASL), Veolia / Texas, USA

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When was the last time you saw a capillary electrophoresis (CE) instrument running in a lab? In the 1990s there was a surge of interest in CE analysis for its potential to revolutionize analytical science which has largely vanished in the 21st century in favor of chromatographic and mass spectrometry systems. CE developed a reputation as being a difficult to understand research tool with poor reproducibility - useful perhaps for solving difficult academic problems but never maturing into a cornerstone of production labs.

Here we showcase the work our Veolia WTS lab has done to overcome some challenges in CE analysis that have allowed it to flourish as one of the most important instruments in our lab. Our lab now runs ~100 samples per week by CE, producing over 20 test results per sample in 10 minutes, and generating virtually no chemical waste or consumption of chemicals/consumables along the way. The technology has proven to be so robust and reproducible, that Veolia WTS now supports the deployment of CE analyzers at customer sites in the field or in smaller satellite labs. The details of this presentation will discuss how we overcame the following challenges to realize this success: (1) shifting and non-reproducible migration times, (2) UV detection for non UV active compounds, (3) difficult data processing, and (4) difficult co-elutions and limited peak capacity. Analytical targets presented include amine compounds, inorganic and organic anions, cationic polymers, and some metals. While it is unrealistic that CE analysis can cover the full space of chemical analysis, we hope this work demonstrates that scientists need to consider CE analysis more often when selecting analytical methods that can meet the criteria of Green Analytical Chemistry. It is possible that the hype begun in the 1990s is still yet to be fully realized.

PFAS Monitoring: Optimizing Analytical Strategies through Non Target
Screening and Passive Sampling Approaches

Gaëla LEROY & Christophe TONDELIER - Veolia Research and Innovations / France

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PFAS are ubiquitous and used in multiple applications due to their chemical properties. They are sadly notorious for their extreme stability and persistence in environmental matrices. This is why Veolia is actively committed to treating these substances in various matrices, placing them at the heart of its depollution strategy.

The impact of PFAS extends to the small water cycle. The contamination of wastewater, particularly due to industrial discharges, can lead to the presence of PFAS in sludge, which may restrict its use in agricultural spreading. Moreover, the discharge of contaminated water can pollute resources used for drinking water production. Thus, numerous studies are currently being conducted to decontaminate water contaminated by these PFAS. These research efforts are exploring the use of ad/absorbing materials such as carbons and resins, or via membrane processes. This challenge is compounded by an increasingly strict regulatory framework. Indeed, currently, only limited lists of substances are monitored due to analytical limitations and lack of knowledge. However, these lists may expand to include broader parameters, notably targeting "total PFAS" in certain geographies.

To anticipate this evolution, Veolia’s department of scientific and technological expertise is conducting in-depth studies on the characterization of PFAS in various matrices, developing protocols for global measurement (total fluorine), and targeted and non-targeted analyses. The proposed presentation aims to illustrate PFAS contamination management through two research projects: one focused on validating a passive sampler designed to track around forty PFAS in sanitation networks to identify their sources and propose actions or solutions for reduction at the source. This validation involves developing analytical methods using liquid and gas chromatography coupled with mass spectrometry (LC-MS and GC-MS). The second project is complementary and aims to expand knowledge on PFAS by establishing a non-targeted screening methodology (NTS: Non-Targeted Screening). This approach is based on analysis by LC coupled with high-resolution MS (LC-HRMS), requiring a complete data processing workflow. This process helps identify PFAS that are still unknown today, with the goal of further deepening contamination characterization.

Whisky analysis by GCxGC under hydrogen

Damien STEYER - Twistaroma / France

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This communication presents an innovative strategy for characterizing volatile compounds in whisky using two-dimensional chromatography (GCxGC) coupled with time-of-flight detection (ToF-MS), with extraction by SPME. The entire setup relies on the use of hydrogen as a carrier gas, in line with green chemistry principles. The objective is twofold: to improve the analytical resolution of key volatile compounds in whisky, while reducing the environmental footprint of the analytical process. The SPME protocol is optimized to maximize the extraction of compounds responsible for the specific aromatic bouquet of whisky, notably esters, phenols, lactones, and sulfur compounds. The GCxGC/ToF-MS configuration allows for comprehensive and reproducible profiles, while identifying subtle olfactory markers not detected by conventional approaches. The use of hydrogen, combined with intelligent management of analytical flows, demonstrates the compatibility between chromatographic performance and sustainability. This study opens up prospects for eco-designed analysis of complex aromatic matrices, with extended applications to other spirits, plant extracts, or fermented products.

Advancements in Solvent Free GCMS Sample Preparation
During the Past 36 Years at Entech Instruments.

Dan CARDIN - Entech / California, USA

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The optimization of sample extraction and delivery to a GCMS follows 2 paths; a few ways to get it right, and hundreds of ways that lead back to the drawing board. A summary is presented of the 36 years of development to create more quantitative collection, extraction and GC delivery of volatiles and semi-volatiles using either zero solvents, or small amounts of low toxicity solvents. Vacuum sampling canisters for VOC collection provided an optimized way to measure the static affinity/partitioning of various chemicals to CVD deposited ceramic surfaces, allowing optimization of coatings to minimize losses of organic compounds prior to reaching the GC. The effects of vacuum on increased cleaning rates of vacuum canister internal surfaces led to the development of direct vacuum extractions of liquid and solid samples, using ceramic coated thermal desorption tubes call Sorbent Pens connected to each sample vial. VASE - Vacuum Assisted Sorbent Extraction, and FEVE – Full Evaporative Vacuum Extraction created a means of transferring chemicals effectively into the Sorbent Pen for either Split or Splitless injection into a GCMS. An all capillary based replacement for multi-bed packed traps was also developed that improves extraction performance, just as capillary GC columns dramatically improved resolution, durability, and consistency compared to earlier packed columns. Individual and hybrid solutions of these new techniques will be presented, with conclusions on where we are now, and where we need to go next.

Development of ionic liquid-based coatings for stir bar sorptive extraction
and application to the non-targeted analysis of emerging organic pollutants
in natural waters via an SBSE-TD-GC–Orbitrap-HRMS method

Pascal CARDINAEL - University of Rouen / Normandie, France

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The monitoring of environmental quality requires regular updates regarding pollutants, particularly emerging ones. Assessing environmental exposure is therefore a crucial step in proposing appropriate protective measures. Most priority pollutants and emerging contaminants are semi-volatile compounds. Non-targeted analysis using gas chromatography coupled with thermal desorption and high-resolution mass spectrometry (TD-GC-HRMS) with an Orbitrap system enables the identification of organic contaminants. This approach also makes it possible to considerably increase the number of compounds identified with high reliability. In this context, a new stir bar sorptive extraction (SBSE) method, using bars prepared with ionic liquid (IL) coatings, was developed. Ionic liquids are salts that are liquid at room temperature, characterized by their unique properties, including high thermal stability, low vapor pressure, and excellent ability to dissolve a wide range of organic and inorganic compounds. Their use should make it possible to broaden the range of detected contaminants and improve the quality of non-targeted screening. This method was applied to natural waters collected from the Robec river in France and two Algerian lakes. A comparison between laboratory-prepared IL-coated bars and commercially available PDMS-coated bars showed a significant increase in the number of compounds detected, accompanied by a notable increase in peak area. In total, more than 1,072 compounds were detected, then classified according to the Miller identification scale, using various scores (RSI, RHRMF, and ΔRI). Moreover, the results obtained made it possible to highlight previously unidentified contaminants.

Overall evolution of the analytical techniques in a water operator laboratory
during the last years towards a green lab

Antonio CABEZA DE LA FUENTE - AGBAR / Spain

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To minimize our environmental impact, we've implemented significant changes and improvements over the past few years, transforming our analytical techniques and laboratory processes. These steps demonstrate our commitment to becoming a green laboratory.

In this way, we have been adapting analytical methods by making the necessary changes, or we have replaced them with alternative methodologies that have allowed us to minimize the amount of hazardous waste generated, which must then be properly managed and treated. These changes have always been aligned with applicable regulatory compliance.

The elimination or limitation of the use of some chemical products and the review of the cleaning processes for materials used in analytical methods have also contributed to the reduction of the amount of hazardous waste generated.

Another line of work developed in recent years is the digitalization of laboratory processes, automating the sending of results from analytical instruments to the laboratory's data manager (LIMS), thus eliminating all primary paper records and improving data traceability. In addition, all laboratory stock control and analytical equipment maintenance operations are managed digitally.

All these changes have been crucial for maintaining our reference certifications and the accreditation under the international standard ISO 17025, ensuring compliance with all legal requirements. As a result, the Aigües de Barcelona laboratory is solidified as a leading reference center, dedicated to environmental protection and committed to a green laboratory model that integrates sustainable practices into all its operations.

Territorial Diagnosis of microplastics from wastewater to drinking water

Lauriane BARRITAUD — VEOLIA - DEST (Department of Scientific and Technical Expertise)

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Two complementary studies conducted by VEOLIA examined microplastic (MP) contamination in aquatic environments. The MEDITPLAST project (2019-2024) investigated Toulon Bay, analyzing MP tyre residues (TR) in various water matrices (stormwater, raw wastewater, treated wastewater …) using specific UFO sampling devices for MP in complex matrices and advanced FT-IR imaging techniques. Results showed wastewater treatment plants achieve up to 99.9% removal efficiency for MP and TR, with tyre residues comprising up to 98% of stormwater contamination. Surprisingly, stormwaters, not treated wastewaters, were the primary source of MP/TR release into the bay.

A parallel study of two French drinking water treatment plants using groundwater employed a dedicated filtration system (STORM) developed by Veolia for sampling large volumes of drinking water (>500 L) on 5 µm stainless steel filters. Results found low MP concentrations in both groundwater and drinking water (<1 MP/L for particles >6.6 µm), with river-influenced groundwater showing higher contamination (2 MP/L) than protected sources (0.3 MP/L). Both studies highlight the high efficiency of water treatment processes while emphasizing the need for harmonized analytical protocols to better understand global MP contamination patterns. these studies were done in collaboration with the University of Aalborg (Jeff Vollertsen)