Herbal-based dietary supplements have become increasingly popular. The extract from milk thistle ( Silybum marianum) , is often used for the treatment of liver diseases. However, serious concerns exist regarding the efficacy, composition, as well as the safety of these over-the-counter preparations. Therefore, the aim of the present study was to investigate the composition as well as chemical and biological safety of 26 milk thistle-based dietary supplements purchased from both the U.S. and Czech markets between 2016 and 2017. The study was focused on a determination of the composition of active ingredients, as well as analyses of possible contaminants including: mycotoxins, plant alkaloids, and pesticide residues, as well as the microbial purity. High-throughput analyses were performed using advanced U-HPLC-HRMS techniques. Large differences in the silymarin content were observed among individual milk thistle preparations, often in contrast with the information provided by the manufacturers. In addition, substantial inter-batch differences in silymarin content were also demonstrated. In all milk thistle preparations tested, large numbers and high concentrations of mycotoxins and several pesticides, as well as the substantial presence of microbiological contamination were detected, pointing to serious safety issues. In conclusion, our results strongly indicate the need for strict controls of the composition, chemical contaminants, as well as the microbiological purity of commercial milk thistle extracts used for the treatment of liver diseases. Poor definition of these preparations together with contamination by biologically active substances may not only account for the inconsistency of clinical observations, but also be responsible for possible herbal-based dietary supplements-induced liver injury.

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Ochratoxin A (OTA) belongs among the most frequently occurring mycotoxins in coffee. In order to investigate its contamination levels in products currently available in the market, a broad set of coffee samples (103 in total) collected between 2016 and 2018 in the Czech Republic was investigated. Aqueous-methanolic extracts purified by using immunoaffinity columns were analysed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (U-HPLC-MS/MS). The undertaken study revealed a relatively low OTA contamination of roasted coffee (in the range 0.2-2.5 μg/kg with the mean concentration of 0.6 μg/kg, and 71% of positive samples). The roasted coffee samples did not exceed the maximum limit of 5 μg/kg set by 1881/2006/EC. With regard to instant coffee samples, OTA concentrations were considerably higher. All the samples were positive, with a mean concentration of 2.9 μg/kg (ranging from 0.6 to 12.8 μg/kg, with 100% of positive samples). One of the analysed samples of instant coffee even exceeded the maximum limit of 10 μg/kg (1881/2006/EC). The study further revealed a relatively high incidence of 14-(R)-OTA, stereoisomer of OTA (14-(S)-OTA), originating as its main degradation product. Its identity was confirmed by high resolution mass spectrometry (HRMS/MS). Most of the samples positive for OTA were also positive for this diastereoisomer, with signal intensities of approx. one-third to one half of the signal of 14-(S)-OTA.

Raw oats are frequently contaminated by fungi producing mycotoxins, and as such, they can pose a health risk to humans regularly consuming oat products. To reveal the effect of particular processing steps on contamination levels in final oat products, two series of samples obtained from an oat flake manufacturer were analysed. Among oat fractions treated, the most significant mycotoxin decrease was demonstrated in cleaning and dehulling steps, where the observed mycotoxin reduction was in the range of 13–75% for monitored mycotoxins, enniatin B, enniatin B1, HT-2 toxin, T-2 toxin, beauvericin and tentoxin. The overall mycotoxin reduction found in final oat flakes was in the range of 65–100%. Furthermore, 20 commercially available oat flakes from the Czech market were analysed. We detected 16 mycotoxins, mainly trichothecenes and emerging enniatins with levels in the interval of 1–156 μg kg^–1. With regard to the current EU legislation, two analysed oat flake products exceeded the maximum limit for ochratoxin A.