In response to the growing demand for rapid, versatile, and sustainable analytical methods in food control, Ambient Pressure Mass Spectrometry (AP-MS) techniques are emerging as innovative and high-performance tools. Among them, Direct Analysis in Real Time (DART) stands out for its ability to analyze samples with minimal sample preparation, reducing analysis time, solvent use, and offering a fast alternative to conventional chromatographic methods by enabling direct ionization under ambient conditions [1]. DART source is typically coupled with High-Resolution MS (HRMS) for food authenticity and safety, while its use with low-resolution MS remains less explored. When combined with a triple quadrupole mass spectrometer (TQ-MS), this platform allows for highly selective and sensitive targeted analysis (MRM mode), suitable for both regulatory and screening purposes. This study presents a rapid, robust, and sustainable analytical method based on DART–TQ-MS/MS applied to two case studies: the detection of adulterated saffron by low-cost spices and the determination of biogenic amines in tuna fish, with a focus on histamine. In the first case study, a rapid and targeted method was developed using an EVOQ triple quadrupole system by monitoring selected the ion transitions 446.4 > 116.2 m/z for safflower, 338.9 > 178.2 m/z for turmeric, enabling the detection of saffron adulteration with safflower and turmeric at levels lower than 5% (w/w). The method was evaluated as satisfactorily green, requiring no toxic solvents and generating minimal waste. The other case study describes the development of a method based on DART-Triple Q MS aimed at determination of histamine in fish products. As well known, histamine is a key safety marker in tuna and other scombroid fish and high levels of histamine could account for an intoxication in sensitive consumers also known as scombroid poisoning. To protect consumer health, EU Regulation (EC) No. 2073/2005 sets a maximum histamine level of 200 mg/kg in fishery products [2]. Optimized MRM transitions 112.2 > 95.0 m/z and 112.2 > 68.1 m/z enabled histamine targeted quantification at level below the enforced limits, confirming the reliability and specificity of the selected markers. The MRM method achieved reliable quantification in compliance with international regulatory limits (EU and FDA) [2], demonstrating its effectiveness for routine safety monitoring. Overall, the DART–TQ–MS/MS platform offers a rapid, versatile, and sustainable approach for assessing food authenticity and ensuring safety in complex matrices.
Application of targeted DART–TQ MS to food safety and authenticity: Two Case Studies
Anna Luparelli;William Matteo Schirinzi;Laura Quintieri;Linda Monaci
2025
Abstract
In response to the growing demand for rapid, versatile, and sustainable analytical methods in food control, Ambient Pressure Mass Spectrometry (AP-MS) techniques are emerging as innovative and high-performance tools. Among them, Direct Analysis in Real Time (DART) stands out for its ability to analyze samples with minimal sample preparation, reducing analysis time, solvent use, and offering a fast alternative to conventional chromatographic methods by enabling direct ionization under ambient conditions [1]. DART source is typically coupled with High-Resolution MS (HRMS) for food authenticity and safety, while its use with low-resolution MS remains less explored. When combined with a triple quadrupole mass spectrometer (TQ-MS), this platform allows for highly selective and sensitive targeted analysis (MRM mode), suitable for both regulatory and screening purposes. This study presents a rapid, robust, and sustainable analytical method based on DART–TQ-MS/MS applied to two case studies: the detection of adulterated saffron by low-cost spices and the determination of biogenic amines in tuna fish, with a focus on histamine. In the first case study, a rapid and targeted method was developed using an EVOQ triple quadrupole system by monitoring selected the ion transitions 446.4 > 116.2 m/z for safflower, 338.9 > 178.2 m/z for turmeric, enabling the detection of saffron adulteration with safflower and turmeric at levels lower than 5% (w/w). The method was evaluated as satisfactorily green, requiring no toxic solvents and generating minimal waste. The other case study describes the development of a method based on DART-Triple Q MS aimed at determination of histamine in fish products. As well known, histamine is a key safety marker in tuna and other scombroid fish and high levels of histamine could account for an intoxication in sensitive consumers also known as scombroid poisoning. To protect consumer health, EU Regulation (EC) No. 2073/2005 sets a maximum histamine level of 200 mg/kg in fishery products [2]. Optimized MRM transitions 112.2 > 95.0 m/z and 112.2 > 68.1 m/z enabled histamine targeted quantification at level below the enforced limits, confirming the reliability and specificity of the selected markers. The MRM method achieved reliable quantification in compliance with international regulatory limits (EU and FDA) [2], demonstrating its effectiveness for routine safety monitoring. Overall, the DART–TQ–MS/MS platform offers a rapid, versatile, and sustainable approach for assessing food authenticity and ensuring safety in complex matrices.| File | Dimensione | Formato | |
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