Quantitative determination of trichothecenes in breadsticks by gas chromatography-triple quadrupole tandem mass spectrometry

Abstract

Breadsticks are pencil-sized sticks of dry bread widely consumed as a pre-meal appetiser. They are basically wheat-based snacks, which makes them a good matrix to evaluate mycotoxin contamination, since wheat is very susceptible to fungal attack. In this sense, the fast, selective and sensitive gas chromatography-triple quadrupole tandem mass spectrometry (GCQqQ-MS/MS) method proposed here allows simultaneous determination of deoxynivalenol (DON), 3-acetyldeoxynivalenol, fusarenon-X, diacetoxyscirpenol, nivalenol, neosolaniol, HT-2 and T-2 toxin in breadsticks after QuEChERS extraction and clean-up. The performance of the method was assessed with respect to European Commission Regulations by studying the selectivity and specificity, limit of detection (LOD), limit of quantitation (LOQ), linearity, matrix effect, accuracy, precision and trueness. Satisfactory results in terms of validation parameters were obtained for all selected mycotoxins (recovery range of 70-110%, RSD < 10%, LOQ <40 µg kg). The trueness of the method was supported by using certified reference material (DON 1062 ± 110 µg kg -1). The method was successfully used to evaluate the occurrence of the studied Fusarium toxins in 61 breadstick samples. A total of 64% of the samples showed mycotoxin contamination, DON being the most frequently detected toxin. Nonetheless, mean levels obtained were far below the maximum levels permitted by European Union legislation. An additional goal was to carry out a risk-characterisation approach to DON by comparing probable daily intake and provisional maximum tolerable daily intake (PMTDI).

Evolution and applications of the QuEChERS method

“…In general, C 18 and PSA are, again, the sorbents most commonly applied in d-SPE, but the combination of these two with Al-N also showed good results [70]. C 18 has been used alone for the extraction of cereals [68,69,73,76], while PSA has been used without C 18 for the extraction of dairy products [67], bee-pollen-based food supplements [71] or cereals [67,70,71,74]. As an example, Fig.…”

“…Rodríguez-Carrasco et al [68] carried out a comparison between MSPD and QuEChERS for the extraction of eight trichotecene mycotoxins from wheat-based breadstick snacks followed by GC-MS/MS analysis. They found that QuEChERS extraction is faster and less laborious, and shows better extraction efficiencies (recoveries higher than 80% in most cases) than MSPD (recoveries of 46-89%).…”

“…Cereals are one of the matrices in which QuEChERS has been most commonly applied and extraction of mycotoxins is no exception -important articles have focused on the extraction of wheat [68,69,72,76], maize [69,72,75,76], soy [69], oat [69], rice [69,70], corn [75,77], and millet [72]. Table 3 shows a representative group of QuEChERS procedures, with sample amounts of 2-15 g being usual, and, since cereals have very low percentages of water, addition of water has also been needed at the beginning of the process [68][69][70][72][73][74][75][76][77].…”

“…The determination of this group of analytes of great concern has been developed exclusively in food analysis [67][68][69][70][71][72][73][74][75], since food is the main route for human exposure. Cereals are one of the matrices in which QuEChERS has been most commonly applied and extraction of mycotoxins is no exception -important articles have focused on the extraction of wheat [68,69,72,76], maize [69,72,75,76], soy [69], oat [69], rice [69,70], corn [75,77], and millet [72].…”

Foodomics in microbiological investigations

“…LC-MS methods were developed for determination of several mycotoxins from food microbes [49 ,50,51]. GC-MS approach is another important tool for foodomics [52][53][54]. CE-MS has been established as a versatile and robust tool providing fast, efficient and automated analytical separation techniques used for food analysis.…”