Cereals represent a widely consumed food commodity that might be contaminated by mycotoxins, resulting not only in potential consumer health risks upon dietary exposure but also significant financial losses due to contaminated batch disposal. Thus, continuous improvement of the performance characteristics of methods to enable an effective monitoring of such contaminants in food supply is highly needed. In this study, an ultra-high-performance liquid chromatography coupled to a hybrid quadrupole orbitrap mass analyzer (UHPLC-q-Orbitrap MS) method was optimized and validated in wheat, maize and rye flour matrices. Nineteen analytes were monitored, including both regulated mycotoxins, e.g., ochratoxin A (OTA) or deoxynivalenol (DON), and non-regulated mycotoxins, such as ergot alkaloids (EAs), which are analytes that are expected to be regulated soon in the EU. Low limits of quantification (LOQ) at the part per trillion level were achieved as well as wide linear ranges (four orders of magnitude) and recovery rates within the 68-104% range. Overall, the developed method attained fit-for-purpose results and it highlights the applicability of high-resolution mass spectrometry (HRMS) detection in mycotoxin food analysis.

• Klíčová slova
• cereal, ergot alkaloids, high-resolution mass spectrometry, mycotoxins, ultra-high-performance liquid chromatography,
• MeSH
• hmotnostní spektrometrie přístrojové vybavení   metody   MeSH
• jedlá semena chemie   MeSH
• kukuřice setá chemie   MeSH
• mouka analýza   MeSH
• mykotoxiny analýza   MeSH
• pšenice chemie   MeSH
• vysokoúčinná kapalinová chromatografie přístrojové vybavení   metody   MeSH
• žito chemie   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• validační studie MeSH
• Názvy látek
• mykotoxiny MeSH

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.

• MeSH
• antioxidancia chemie   fyziologie   MeSH
• biologické přípravky chemie   farmakologie   MeSH
• fytoterapie metody   MeSH
• lidé MeSH
• mykotoxiny chemie   MeSH
• nemoci jater farmakoterapie   MeSH
• ostropestřec mariánský chemie   mikrobiologie   MeSH
• pesticidy chemie   MeSH
• potravní doplňky mikrobiologie   MeSH
• rostlinné extrakty chemie   farmakologie   MeSH
• silymarin chemie   farmakologie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• antioxidancia MeSH
• biologické přípravky MeSH
• mykotoxiny MeSH
• pesticidy MeSH
• rostlinné extrakty MeSH
• silymarin MeSH