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. Screening of plant toxins in food, feed and botanicals using full scan high resolution (Orbitrap) mass spectrometry. Food Additives and Contaminants, 2011, 28 (10), pp.1405-1423. <10.1080/19440049.2011

Flow injection combined with tandem mass spectrometry (MS/MS) was investigated for the rapid detection of highly polar pesticides that are not amenable to multi-residue methods because they do not partition into organic solvents and require dedicated chromatographic conditions. The pesticides included in this study were amitrole, chlormequat, cyromazine, daminozide, diquat, ethephon, fosetyl-Al, glufosinate, glyphosate and its metabolite aminomethylphosphonic acid, maleic hydrazide, mepiquat and paraquat. The composition of the flow-injection solvent was optimized to achieve maximum MS/MS sensitivity. Instrumental limits of detection varied between <0.05 and 1 pg. Fruit, vegetable, cereal, milk and kidney samples were extracted with water (1% formic acid in case of paraquat/diquat) and ten times diluted in either methanol/0.1% formic acid, methanol/0.1% ammonia or acetonitrile/0.1% ammonia, depending on the pesticide. The ion suppression observed depended strongly on both the matrix and the pesticide. This could be largely compensated for by matrix-matched calibration, but more accurate quantification was obtained by using isotopically labelled standards (commercially available for most of the pesticides studied). The method detection limits ranged from 0.02 mg/kg for chlormequat and mepiquat to 2 mg/kg for maleic hydrazide and were 0.05-0.2 mg/kg for most other pesticide/matrix combinations. This was sufficiently low to test compliance with EU maximum residue limits for many relevant pesticide/commodity combinations. The method substantially reduces the liquid chromatography-MS/MS capacity demand which for many laboratories is prohibitive for inclusion of these pesticides in their monitoring and surveillance programmes.

In 2017, a Total Diet Study was conducted in the Netherlands in which mycotoxins were analysed in foods and beverages consumed by 1- and 2-year-old children. These mycotoxins were aflatoxins, Alternaria toxins, citrinin, ergot alkaloids, fumonisins, ochratoxin A, patulin, sterigmatocystin, trichothecenes, and zearalenone. Long-term exposure was calculated by combining concentrations in foods and beverages with consumed amounts of these products. Analysed foods and beverages with a concentration below the detection limit that could contain the mycotoxin, were assigned a concentration equal to half this limit value. To assess if the exposure could result in a possible health risk, the high long-term exposure (95th percentile) was compared with a health-based guidance value (HBGV) or a margin of exposure (MOE) was calculated. Exposure to aflatoxins, Alternaria toxins, ochratoxin A and T-2/HT-2 sum may pose a health concern. Foods that contributed most to the exposure of these mycotoxins were bread, biscuits, breakfast cereals, chocolates, dried fruit, follow-on formula and fruit juices.