15 Environmental Analysis & Electrochemistry


These approaches continue to be refi ned in the latest LC-MS/MS technologies. For instance, a new triple quadrupole mass spectrometer has been engineered to maintain the optimal sensitivity performance for up to twice as long as compared with existing SCIEX technology, particularly when running complex matrices.[14,15] The SCIEX 7500+ system is the fastest scanning SCIEX triple quadrupole system so far and can acquire up to 800 MRM transitions per cycle, increasing the scope for large quantitation panels that incorporate new compounds of concern.[14] An LC-MS/MS analysis using a simplifi ed QuEChERS protocol and MRM quantitation on the SCIEX 7500+ system achieved LOQs for all the mycotoxins and tropane alkaloids tested that were 10–250 times lower than the lowest MRLs required by EU legislation.[11] The LOQs for mycotoxins such as afl atoxins and ochratoxin A in cereal-based products were in the


sub-parts per billion (ppb) range, well below the regulatory limits set for these matrices. [5,11] Similarly, in dairy products and infant food, where MRLs were stricter, the SCIEX 7500+ system achieved LOQs well below these regulatory thresholds (see Figure 2).[5,11] The high sensitivity of the MS system enabled a small injection volume of 1.5 μL, while still capable of sub-ppb detection, resulting in low carry-over. The method demonstrated accurate and highly reproducible quantitative performance for all compounds in baby food, almond, grape juice, and wine matrices.


The system has demonstrated increased resilience in analysing a large range of sample types and workfl ows, under the most extreme conditions.[14] This is partly due to the inclusion of an innovative proprietary technology, Mass Guard technology, which actively fi lters out potentially contaminating ions. This reduces the risk and frequency of instrument contamination.[15,16] Another refi nement is the newly designed DJet+ assembly, which is fully removable and can be cleaned and maintained by users, making it easier to schedule front-end cleaning and maximise system uptime.[14,15]


The SCIEX 7500+ system is enabled with QTRAP technology, which combines the capabilities of a triple quadrupole MS with a linear ion trap (LIT) for simultaneous quantitation and qualitative identifi cation.[11,18] For example, as part of the QTRAP functionality, the MRM3 workfl ow provides enhanced specifi city for analyte detection in complex matrices like baby food (see Figure 3). The dual fragmentation of analyte precursor ions results in the production of fi rst- and second-generation product ions, yielding more unique and compound-specifi c MRM3 transitions for monitoring. This increased specifi city enables the removal of co-eluting matrix interferences, which can improve signal-to-noise and LOQ selection due to a cleaner chromatographic background.[11,18]


Figure 3: Comparison of MRM and MRM3 scan XICs of blank and low-level standards for afl atoxin B2 in baby food matrix. The XICs show that the MRM scan for afl atoxin B2 in baby food contains an interference, indicated in the matrix blank, and results in accurate quantitation not being possible below 0.0625 µg/kg. MRM3 provides an alternative solution when MRM-based quantitation is hindered by high background and co-eluting interferences. The increased specifi city of the MRM3 scan removed the interference peak from the matrix blank, resulting in a lower LOQ of 0.0025 µg/kg for afl atoxin B2.[11,18] Credit: SCIEX.


Figure 2: A: XICs of four mycotoxins in the matrix blank (fi rst row) and in baby food pre-spiked at the LOQ. Quantifi er ion is shown in blue, fi rst qualifi er ion is shown in pink. Using the SCIEX 7500+ system, LOQ values of 0.01 μg/kg were achieved for afl atoxin, 0.0625 μg/kg for afl atoxin B2, 0.2 μg/kg for HT-2 toxin, and 0.03 μg/kg for ochratoxin A. These values are 10–250 times lower than the MRL values required in regulation EC 2023/915 for these specifi c mycotoxins in baby food matrix.[5,11]


With stringent regulations governing toxin levels in food and feed, analytical technologies must ensure compliance with international standards set by agencies such as the European Food Safety Authority (EFSA), the US Food and Drug Administration (FDA), and the Codex Alimentarius. Developers of advanced tools like the SCIEX 7500+ system provide methods that have been optimised to align with regulatory requirements, delivering ultrafast and highly sensitive MRM acquisition for multiresidue analysis.[11,15,17]


Mass spectrometry innovations help food safety keep pace with changing environment


The impact of climate change on mycotoxin, masked mycotoxin, and tropane alkaloid contamination presents a formidable challenge to global food safety. Rising temperatures and shifting weather patterns are driving an increase in fungal proliferation and the spread of toxic plant species, necessitating advanced analytical solutions to mitigate risks. Mass spectrometry and portable detection technologies are revolutionising toxin analysis by offering high sensitivity and rapid multi-residue screening.


As the food industry adapts to the evolving threats posed by climate change, continued innovation in analytical testing will play a vital role in ensuring food safety. Laboratories equipped with cutting-edge MS systems and other advanced analytical platforms can provide accurate and reliable detection of current and emerging contaminants of concern. The integration of these technologies into routine food safety testing can help mitigate risks, futureproof against evolving regulatory changes, and protect from the growing threats posed by climate change.


References


1. Kos J, Anić M, Radić B, et al. Climate Change—A Global Threat Resulting in Increasing Mycotoxin Occurrence. Foods 2023;12:2704. doi: 10.3390/foods12142704.


2. Eyre D. National Plant Health Week: extreme weather and plant pests. GOV.UK Environment Blog post. May 7, 2024. Available at: https://defraenvironment.blog.gov.uk/2024/05/07/national-plant-health-week- extreme-weather-and-plant-pests/. Accessed March 7, 2025.


3. Jank B, Rath J. Emerging tropane alkaloid contaminations under climate change. Trends Plant Sci. 2021;26:1101–3. doi: 10.1016/j.tplants.2021.08.001.


4. mStahl-Zeng J, Fillâtre Y, McMillan D, Taylor P, Moore I. Robust, high-throughput, fast polarity switching quantitation of 530 mycotoxins, masked mycotoxins and other metabolites. SCIEX Technical Note. Available at: https://sciex.com/content/dam/SCIEX/pdf/tech-notes/food-and-beverage/food-and-beverage/Fast- polarity-switching_530-Mycotoxins_5500+_%20RUO-MKT-02-9463-A.pdf. Accessed February 27, 2025.


Figure 2: B: LOQ values achieved for mycotoxins in 4 food matrices using standard MRM workfl ow, compared with the lowest MRL value required by Regulation EU 2023/9151, EU 2024/10382 and Recommendation EU 2022/5533.[11] Credit: SCIEX.


LC-MS/MS offers the benefi t of comprehensive multi-residue screening. Contamination often involves the co-occurrence of multiple toxins and other endogenous components in a single sample, which necessitates an analytical approach that can simultaneously quantify various contaminants and resolve them from matrix interferences.


5. Document 02023R0915-20250101. Consolidated text: Commission Regulation (EU) 2023/915 of 25 April 2023 on maximum levels for certain contaminants in food and repealing Regulation (EC) No 1881/2006 (Text with EEA relevance).. Available at: https://eur-lex.europa.eu/legal-content/EN/ TXT/?uri=CELEX%3A02023R0915-20250101. Accessed March 7, 2025.


6. Commission Regulation (EU) 2021/1408 of 27 August 2021 amending Regulation (EC) No 1881/2006 as regards maximum levels of tropane alkaloids in certain foodstuffs (Text with EEA relevance). Available at: https://eur-lex.europa.eu/eli/reg/2021/1408/oj/eng. Accessed February 27, 2025.


7. Ahuja V, Singh A, Paul D, et al. Recent Advances in the Detection of Food Toxins Using Mass Spectrometry. Chem Res Toxicol. 2023;36:1834–63. doi: 10.1021/acs.chemrestox.3c00241.


8. Wang Y, Zhang C, Wang J, Knopp D. Recent Progress in Rapid Determination of Mycotoxins Based on Emerging Biorecognition Molecules: A Review. Toxins (Basel). 2022;14:73. doi: 10.3390/toxins14020073.


9. Singh J, Mehta A. Rapid and sensitive detection of mycotoxins by advanced and emerging analytical methods: A review. Food Sci Nutr. 2020;8:2183–2204. doi: 10.1002/fsn3.1474.


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