Innovations in Food Safety: Cutting-Edge Analytical Tests and Techniques

1.0 Introduction

Food testing laboratories are essential for ensuring both the safety and authenticity of food products within the increasingly complex global food supply chain. Accurate quantification of pesticide and antibiotic residues is critical for food safety and compliance with international trade regulations. Additionally, anthropogenic contaminants, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and per- and polyfluoroalkyl substances (PFAS), as well as other hazardous substances such as dioxins and furans, pose significant risks due to their potential for bioaccumulation and carcinogenicity. Regulatory frameworks at both the global and national levels establish maximum residue limits (MRL) or tolerance limits (TL) for these compounds. Tandem mass spectrometry is recognized as the benchmark for compliance testing when analysing residues and contaminants listed in target lists across various food matrices. Despite considerable progress in recent times, these conventional residue and contaminant testing activities generate substantial waste, including organic solvents, sorbents, and plasticware. Additionally, diverse groups of naturally occurring toxins and emerging organic contaminants may be present in food and pose a significant challenge for food testing laboratories operating under a target list-based testing regime. Economically motivated adulteration (EMA) and mislabelling of food products also pose significant new challenges to food safety and authenticity, particularly where traditional testing methodologies fall short.

New analytical tests and techniques are being developed to address these emerging challenges to food safety and authenticity. Large-scope analytical methods are being developed to simultaneously quantify the maximum number of residues and contaminants possible in food. Several innovations in the sample preparation, including online automated sample preparation with the instrument, are being developed to improve the green metrics of the analytical methods. Analytical methods for food authenticity determination have also seen rapid growth, supported by innovations in instrumentation and artificial intelligence. This article presents a brief overview of these emerging techniques in food safety and authenticity determination.

2.0 Green Analytical Techniques in Residue and Contaminant Analysis

The latest trend in residue and contaminant analysis is the development of generic methods capable of monitoring a wide variety of compounds belonging to different chemical classes. This has proven challenging due to the varying chemistries and physicochemical properties. Recently, the FSSAI-NRLs of fish and fisheries products and fruits and vegetables reported a large-scope multiresidue method for the analysis of 380 microchemicals, including pesticides and antibiotics, in fish, poultry meat, and eggs (Nazar et al., 2025). The NRL on fruits and vegetables at ICAR-NRC Grapes has also recently expanded its scope of accreditation to include multiresidue testing of 779 pesticides covering almost all compounds having relevance for the country. Another study reports an analytical method using a high-resolution mass spectrometer for screening and quantification of >1100 pesticides and natural toxins in cereal products (Bessaire et al., 2024). The trend suggests an increasing use of high-resolution mass spectrometers and large-scale screening of residues and contaminants in foods to identify emerging contaminants not covered by traditional target-list-based regulatory testing. In comparison, multi-class methods for veterinary drugs are still not so widespread, although those are strongly required.

2.1 Miniaturized Solid-Phase and Liquid-Phase Extraction Techniques

The principal methodologies that align with the principles of green analytical chemistry (GAC) predominantly involve advanced miniaturized solid-phase extraction (SPE) techniques. Key approaches include microextraction in packed syringes (MEPS), solid-phase microextraction (SPME) implemented in both direct immersion (DI) and headspace (HS) formats, stir-bar sorptive extraction (SBSE), and matrix solid-phase dispersion. In addition, several innovative liquid-phase extraction strategies have emerged as environmentally benign alternatives. These comprise single-drop microextraction, hollow fibre liquid-phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME), QuEChERS, solidification of floating organic drop microextraction (SFOME), and ultrasound-assisted back extraction (UABE) (Dugheri et al., 2021; Moyo et al., 2022; Jagirani et al., 2022).

2.2 Green Solvents

Green solvents (GSs) have frequently been integrated with these extraction techniques to enhance the efficient and sustainable recovery of target antibiotic residues. GSs such as supramolecular solvents (SUPRAS), ionic liquids (ILs), and deep eutectic solvents (DES) are finding increasing application in the extraction of antibiotic residues. In particular, DES shows significant potential for antibiotic extraction, as evidenced by a growing body of literature (Shahi et al., 2022; Saei et al., 2020; Saei et al., 2022).

2.3 Environmentally Sustainable Sample Preparation

In recent years, there has been a significant shift towards environmentally sustainable sample preparation techniques, moving away from conventional Soxhlet extraction. Techniques such as ultrasonication-assisted extraction (UAE) and microwave-assisted extraction (MAE) have gained traction, alongside advanced methodologies like pressurized liquid extraction (PLE) and supercritical fluid extraction (SFE). These innovative approaches not only enhance extraction efficiencies but also minimize solvent consumption, thereby aligning with current sustainability objectives within analytical chemistry. MAE has been used for rapid extraction of pharmacologically active substances from animal tissue (Rodríguez-de Cos et al., 2024; Santana-Viera et al., 2023). A multiresidue analysis of tetracyclines and β-receptor agonists in chicken was developed using PLE followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination (Wang et al., 2020).

2.4 Chromatographic Techniques and Supercritical Fluid Chromatography

Liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS) continue to be the benchmark techniques for analyzing intricate matrices. Furthermore, supercritical fluid chromatography (SFC), which employs carbon dioxide as the mobile phase, emerges as a robust process within the realm of green analytical chemistry. SFC provides significant advantages, particularly in minimizing hazardous organic solvent usage by utilizing a non-toxic, eco-friendly solvent system. Furthermore, this technique enhances chromatographic separation efficiency, positioning it as a highly attractive option for contemporary analytical applications.

A comparative study assessing the separation efficacy of SFC against serial reverse-phase and hydrophilic interaction liquid chromatography (RP-HILIC) involved the analysis of 274 environmentally relevant compounds. When integrated with time-of-flight mass spectrometry (TOF-MS), both methodologies proved effective for hidden-target screening in environmental wastewater samples (Bieber et al., 2017). Additionally, the SFC-MS technique has been successfully employed to analyze multi-class pesticides across various food matrices, demonstrating its versatility and analytical power (Ishibashi et al., 2015; Tao et al., 2018).

3.0 Advanced Analytical Techniques in Food Authenticity Determination

Food authenticity encompasses the integrity and verifiable characteristics, origin, and identity of food products, alongside their compliance with expected attributes. Unfortunately, the intricate nature of the global food supply chain has enabled the infiltration of fraudulent practices, leading to significant authenticity challenges. These issues contribute to annual losses estimated at around US $40 billion for the food industry.

3.1 DNA-Based and Spectroscopic Methods

In recent years, advanced analytical techniques have been increasingly employed to address concerns about food authenticity. Methods such as DNA barcoding and Next Generation Sequencing (NGS) have proven particularly effective for verifying the species identity of agricultural commodities. Additionally, Metabolomics Fingerprinting Leveraging High-Resolution Mass Spectrometry (HRMS) and Nuclear Magnetic Resonance (NMR) spectroscopy has shown considerable promise in authenticating geographical provenance and detecting complex food adulteration, particularly in honey. Furthermore, peptide biomarkers are being explored for their potential in enhancing food authenticity verification.

3.2 Ambient Mass Spectrometry (AMS) Techniques

Ambient mass spectrometry (AMS) techniques represent recent innovations in analytical chemistry. They require little or no sample preparations and significantly reduce the time required for the sample analysis. Moreover, AMS techniques offer comparable results with the traditional mass spectrometry techniques in terms of specificity, sensitivity, and resolution (Black et al., 2016). This comprises a range of sophisticated techniques including:

• Paper spray mass spectrometry (PS-MS)
• Direct analysis in real-time mass spectrometry (DART-MS)
• Desorption electrospray ionization (DESI-MS)
• Atmospheric analysis probe (ASAP-MS)
• Rapid evaporative ionization mass spectrometry (REIMS)
• Liquid extraction surface-mass spectrometry (LESA-MS)
• High-voltage-assisted laser desorption ionization-mass spectrometry (HALDI-MS)

Out of the various AMS techniques, DART-MS, REIMS, DESI-MS, and ASAP-MS are the commonly used methods for the rapid authentication of food samples (Black et al., 2016). These techniques enable the swift and direct analysis of samples in ambient conditions, simplifying the sample analysis process. AMS methods facilitate high-speed and high-throughput sample analysis, as they eliminate the need for extensive sample preparation.

4.0 Conclusion

Globalizing the food supply chain presents unique challenges to food safety and food authenticity. Target list-based monitoring of residues in food is often inadequate in globalised supply chains. Hence large-scope screening and quantitation methods are necessary. Companies often substitute expensive ingredients with cheaper alternatives or misbrand products with misleading geographic claims, undermining consumer trust and posing public health risks. To address these issues, advancements in detection technologies are crucial. Techniques such as chromatography and mass spectrometry help verify food safety and authenticity by identifying key constituents and metabolites. Recently, deep learning methods, including multilayer perceptrons (MLP) and convolutional neural networks (CNN), have enhanced the assessment of food quality and visual attributes. Other models like recurrent neural networks (RNN), autoencoders (AE), and generative adversarial networks (GAN) also show promise in this field. As technology continues to advance, deep learning can provide quicker and more accurate food identification, ultimately offering consumers safer food options and fostering progress in the food sector.

References

Author Biography