Tackling Food Fraud with “Chromatography-Free” Mass Spectrometry

Economically motivated adulteration (EMA) is a growing global issue that not only threatens food producers and the food supply chain, but could also have a damaging impact on human health. EMA involves the deliberate introduction of inferior substances in food products with the intention of increasing quantity, reducing production costs, or creating an imitation of a high-value product. EMAs are designed to avoid detection, and establishing the presence of adulterants in food samples is a major challenge for the food industry.

The number of cases of EMA has escalated dramatically over the last five years, with a recent report indicating a 1041% increase in incidents from 2020 to 2023.¹ While the exact economic impact is difficult to determine, the U.S. Food and Drug Administration (FDA) estimates that food fraud costs the global food industry between $10 billion and $15 billion annually.² Alongside its financial implications, EMA can pose a serious threat to human health as adulterated foods can contain toxic chemicals or undeclared allergens. It is therefore essential that effective adulterant detection methods are implemented to tackle food fraud.

The Italian National Research Council (CNR) is the largest public research institution in Italy, supporting scientific and technological innovation across the country. The Mass Spectrometry team at the CNR Institute of Biomembranes, Bioenergetics and Molecular Biotechnologies (IBIOM), located in Bari, Italy, has developed a new chromatography-free method, using direct analysis in real time (DART) coupled with triple quadrupole mass spectrometry (QqQ), to help protect and maintain high levels of food quality in Europe.

Limitations of Chromatographic Methods

Methods for food sample analysis have evolved considerably in recent years. Chromatographic methods that were once coupled with fluorometric (FL) or ultraviolet (UV) detectors are now typically used in conjunction with mass spectrometry (MS). Due to its high analytical potential, MS has become a leading analytical technique for food quality control (QC) and for the detection and quantification of a range of contaminants. This technique provides highly sensitive and specific results and has been used to identify unknown compounds, determine molecular weight, and quantify known materials. Some interesting results have also been obtained in the detection and quantification of chemical contaminants and adulterants in food samples.

Despite widespread use across the food-testing community, chromatographic methods have distinct limitations: They often require long analysis times and employ medium-large volumes of organic solvents that are classified as hazardous waste and require proper disposal. A fast, more environmentally friendly method for reliable food quality control is needed to tackle the growing threat of EMA.

Accelerating Quality Control With DART-MS

Direct analysis in real time mass spectrometry (DART-MS) has emerged as an effective “chromatography-free” alternative for rapid detection or confirmation of adulterants in food samples. It represents a paradigm shift from targeted, labor-intensive analytical chemistry toward rapid, non-destructive, high-throughput screening methodologies.

The CNR-IBIOM Mass Spectrometry Unit, working under the guidance of Linda Monaci, has developed an innovative and simple DART-MS/MS workflow for qualitative analysis of food samples, which is being expanded to different food products. The optimized workflow requires quick and minimal sample preparation before using DART, an ambient ionization technique that allows direct ionization of samples in open air, followed by rapid mass spectral analysis. Combining DART and triple quadrupole mass spectrometry (QqQ) also allows the unit to harness the speed of the DART acquisition time and the selectivity of multiple reaction monitoring (MRM) in a “chromatography-free” workflow. Such considerable time savings facilitate the acquisition of the large datasets required for thorough adulterant analysis. The unit can then use exception-based data review software and automated sample reporting to process the datasets efficiently and rapidly confirm the presence of adulterants in food samples.

Researchers in the food testing arena are also working to reduce the environmental impact of their methods, and the CNR-IBIOM Mass Spectrometry Unit is no exception. DART-MS provides improvements in lab sustainability as it minimizes the use of organic solvents, removing up to 95% of organic waste in select applications.

Detecting Saffron Adulteration

Valued at between $1,100 and $11,000 per kilogram, saffron is an expensive spice harvested by hand from Crocus sativus L.³ As a result, saffron commands a premium price, and is frequently targeted by fraudsters who illegally add substances, such as safflower and marigold powder, to increase the yield of their products as a way to boost profit per kilo.

Gas chromatography mass spectrometry (GC–MS) and liquid chromatography mass spectrometry (LC–MS) are typically used by food-testing scientists to detect saffron adulteration, but analysis using these methods can be complex and lengthy, delaying time-sensitive results. The current official standard method is UV-Vis spectroscopy coupled with high-performance liquid chromatography (HPLC); although it provides a high level of accuracy, it cannot detect saffron adulterants at levels below 20%. This presents a challenge to testing labs, as fraudsters often introduce adulterants at low levels to avoid detection.

Recognizing the limitations of existing methods, the CNR-IBIOM Mass Spectrometry Unit has developed a robust, high-throughput detection method using DART-MS to quickly and accurately detect saffron samples adulterated with safflower. First, the unit performed MS scan experiments to select the precursor ions that would act as markers to trace the safflower. A product ion scan then allowed identification of the most reproducible and intense MRM transitions of the pre-selected markers, and collision energy optimization enhanced the method sensitivity. Both the MS and DART settings were optimized for DART tandem mass spectrometry (DART–MS/MS) analysis. An internal standard (IS) introduced to optimize the MRM method significantly improved the reproducibility of the analysis. Following an assessment of the calibration curves of real samples, the unit applied the workflow to an existing case of adulterated saffron.

The new workflow is now in regular use at the CNR-IBIOM Mass Spectrometry Unit lab and has dramatically improved both the speed and the sensitivity of saffron adulteration analysis. Quick and easy sample preparation has been a key benefit: The time required for saffron extraction and analysis can be as short as 10–15 min using a mixture of water and ethanol, resulting in significant time savings. Overall, MS analysis time is short, at approximately 20 s per sample, compared with 6–7 min for LC analysis. DART-MS can achieve the sensitivity needed for the analysis of saffron samples. Unlike UV-VIS spectroscopy HPLC, DART-MS allows the team to identify safflower contamination in saffron samples at levels as low as 5%, a vast improvement over the official standard method.

Unlocking New Applications in Food Testing

The CNR-IBIOM Mass Spectrometry Unit is also working to expand its DART-MS method for broader food analysis applications, including allergen screening and contaminant detection. For example, recent experiments have centered around optimizing the conditions for the detection of markers of histamine in foods. Alongside this, the unit has highlighted the potential of DART-MS to detect and quantify toxic compounds, such as biogenic amines and mycotoxins.

DART-MS is already playing a key role in the ongoing fight against EMA and its suitability for wider food applications promises to cement its position as a crucial tool for food authenticity analysis in labs across the globe.

References
1. Food Fraud Explosion: A Tenfold Increase from 2020 to 2024—Predictions and Prevention Strategies. Digicomply. https://www.digicomply.com/blog/food-fraud-explosion (accessed Feb 10, 2026).

2. Economically Motivated Adulteration (Food Fraud). U.S. Food and Drug Administration. https://www.fda.gov/food/compliance-enforcement-food/economically-motivated-adulteration-food-fraud (accessed Feb 10, 2026).

3. Saffron. ChemEurope. https://www.chemeurope.com/en/encyclopedia/Saffron.html (accessed Feb 11, 2026).