Methodological developments in the sampling of foods and feeds for mycotoxin analysis (original) (raw)

www.mdpi.com/journal/ijms/ An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins

2009

Abstract: Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass s...

Qualitative and Quantitative Analysis of Mycotoxins

Comprehensive Reviews in Food Science and Food Safety, 2009

Mycotoxin toxicity occurs at very low concentrations, therefore sensitive and reliable methods for their detection are required. Consequently, sampling and analysis of mycotoxins is of critical importance because failure to achieve a suitable verified analysis can lead to unacceptable consignments being accepted or satisfactory shipments unnecessarily rejected. The general mycotoxin analyses carried out in laboratories are still based on physicochemical methods, which are continually improved. Further research in mycotoxin analysis has been established in such techniques as screening methods with TLC, GC, HPLC, and LC-MS. In some areas of mycotoxin method development, immunoaffinity columns and multifunctional columns are good choices as cleanup methods. They are appropriate to displace conventional liquid-liquid partitioning or column chromatography cleanup. On the other hand, the need for rapid yes/no decisions for exported or imported products has led to a number of new screening methods, mainly, rapid and easy-to-use test kits based on immuno-analytical principles. In view of the fact that analytical methods for detecting mycotoxins have become more prevalent, sensitive, and specific, surveillance of foods for mycotoxin contamination has become more commonplace. Reliability of methods and well-defined performance characteristics are essential for method validation. This article covers some of the latest activities and progress in qualitative and quantitative mycotoxin analysis.

Towards harmonized approaches for mycotoxin analyses: an assessment

Quality Assurance and Safety of Crops & Foods, 2009

Mycotoxins (the poisonous metabolites of certain filamentous fungi) are potential contaminants of staple food commodities and, if uncontrolled, may present a significant public health hazard. In many jurisdictions, questions relating to mycotoxin contamination are addressed at both generic and specific levels by food-safety legislation. Key to the successful management of the mycotoxin question, both in terms of verifying food-safety measures by the agri-food businesses and ensuring compliance with statutory limits by enforcement agencies, is the use of reliable sampling and analytical methodology. Evidence from European Union Rapid Alert System for Food and Feed data suggest that harmonization of methodologies used to determine the mycotoxin content of foods would contribute to improved compliance at both regulatory and commercial levels.

An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins

International Journal of Molecular Sciences, 2009

Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass spectrometric detection, while in the field of sample preparation various solid-phase extraction approaches are discussed. However, an overview of other analytical and sample preparation methods less often used is also given. Finally, different matrices where mycotoxins have to be determined are discussed with the emphasis on their specific characteristics important for the analysis (human food and beverages, animal feed, biological samples, environmental samples). Various issues important for accurate qualitative and quantitative analyses are critically discussed: sampling and choice of representative sample, sample preparation and possible bias associated with it, specificity of the analytical method and critical evaluation of results.

Simultaneous multiple mycotoxin quantification in feed samples using three isotopically labeled internal standards applied for isotopic dilution and data normalization through ultra-performance liquid chromatography/electrospray ionization tandem mass spe

Rapid Communications in Mass Spectrometry, 2012

RATIONALE: Mycotoxins are typically present in grain and are also concentrated in distillers dried grains with solubles (DDGS), common feed ingredients for food animals. The diversity of mycotoxins and feed matrices has made the routine detection and quantification of mycotoxins in feed both complex and prohibitively expensive. METHODS: Ultra-performance liquid chromatography/electrospray ionization triple quadrupole detection (UPLC/ESI-TQD) (tandem mass spectrometry, MS/MS) with 13 C-labeled isotopic dilution was used to analyze internal standard isotopologues of three mycotoxin molecules, as well as 29 other structurally differing mycotoxin molecules from four common feed matrices: corn, wheat, barley, or DDGS. Mycotoxins were extracted via a single-step procedure using a mixture of acetonitrile/water/formic acid. Labeled isotopologues were used as a surrogate to account for extraction quality and as internal standards for the evaluation of the feed matrix signal suppression/enhancement (SSE) contributed by each mycotoxin and by each matrix. The SSE was corrected by matrix-matched calibration with blank certified reference feed material. RESULTS: The limits of detection for individual mycotoxins in buffer ranged from 0.01 to 206.7 mg/mL but could increase by up to four times depending on the matrix effect. The accuracy and precision were enhanced by the use of isotopically labeled standards. The recoveries were somewhat negatively affected by the SSE contributed by each matrix. Each mycotoxin was successfully detected and assigned to one of four SSE categories: high (-66%), intermediate (-48%), low (-19%) signal suppression and signal enhancement (> +300%). CONCLUSIONS: An improved LC/MS method was validated, which offers a practical and economical means for large-scale detection and quantification of multiple mycotoxins in common animal-feed matrices, including DDGS.

The use of mycotoxin methodology in practice: a need for harmonization

Quality Assurance and Safety of Crops & Foods, 2009

Background In the EU, sampling and analysis for the official control of the levels of mycotoxins in foodstuffs should be performed in accordance with the methods and criteria set out in Commission Regulation 401/2006. For each mycotoxin, the values of recovery, repeatability and reproducibility of the analytical method selected by each laboratory must fall within the range of acceptability as prescribed in the Regulation. Aims Carry out a survey on current practices concerning the use and application of mycotoxin test methods for what are considered to be the most current commercially significant mycotoxins. Materials and Methods Nineteen control, commercial and research laboratories from 12 countries (United Kingdom,

Analysis of naturally occurring mycotoxins in feedstuffs and food

Journal of animal science, 1993

Aflatoxins, zearalenone, deoxynivalenol, fumonisins, and their respective metabolites require specific procedures for their determination because of their diverse chemistry and occurrence in complex matrices of feedstuffs and foods. Major sources of error in the analysis of these mycotoxins arise from inadequate sampling and inefficient extraction and cleanup procedures. The determinative step in the assay for each of these toxins is sensitive to levels below those that are considered detrimental to humans and animals. Aflatoxins can be determined in grains and animal fluids and tissues by TLC, HPLC, gas chromatography-mass spectrometry (GC-MS), and ELISA procedures. Zearalenone, an estrogenic mycotoxin, can readily be determined in cereal grains and foods by HPLC (50 ng/g) and by TLC (300 ng/g). No incurred levels of zearalenone or its metabolites have been detected in animal tissues destined for human consumption. Deoxynivalenol can be determined in wheat and corn at 300 ng/g by a...

Principles of risk assessment of mycotoxins in food and feed

2013

MYCOTOXINS: A REVIEW OF REGULATORY ASPECTS There are several international organizations with scientific boards dealing with the problem of food and feed contaminants. Apart the International Agency for Research on Cancer (IARC, Lyon, France) which is focused on carcinogenicity of natural and manmade compounds, there is also a more recently founded (1980) International Programme on Chemical Safety (IPCS), a joint venture of the United Nations Environmental Programme (UNEP), the International Labour Organization (ILO) and WHO. IPCS organizes scientific meetings of experts called Joint FAO/WHO Expert Committees on Food Additives (JECFA) which is particularly concerned about the safety of food additives, residues of veterinary drugs, naturally occurring toxicants and contaminants of food. JECFA serves as scientific advisory body to FAO, WHO, their Member States and the Codex Alimentarius Comission. In order to protect European consumers from the exposure of all kinds of possible lesions and diseases of food origin the European Commission (EC) founded the independent scientific advisory board called European Food Safety Authority (EFSA) 1. In 2003, EFSA organized Panel on Contaminants in the Food Chain (CONTAM Panel) with the mandate to deliver scientific opinions on-contaminants in food and feed, associated areas and undesirable substances such as natural toxicants, mycotoxins and residues of non-authorized substances not covered by another Panel‖. CONTAM Panel receives the requests from the EC (95 %), Member States (1 %) and the European Parliament (1 %). Since 2003 CONTAM Panel produced 107 opinions (55 on contaminants in food, 43 in feed and 9 combined assessments in food and feed), 15 out of them on mycotoxins. Evaluation of risk assessment of mycotoxins is specific because of their natural origin and it relies on public scientific information. Mycotoxins are secondary metabolites produced by many species of filamentous fungi. Around 300 different mycotoxins have been described that are produced by about 200 different fungal species. However, there are only 20 mycotoxins that are regularly found in food and feedstuffs at concentrations likely to pose a health hazard for animals and people consuming these materials-socalled-primary exposure‖. The commonly known and health relevant mycotoxins can be categorized into Aspergillus mycotoxins (e.g. aflatoxins, ochratoxins), Fusarium mycotoxins (e.g. fumonisins, trichothecenes, zearalenone, nivalenol, deoxynivalenol, T-2 toxin, enniatins and beauvericin) and Penicillium mycotoxins (e.g. ochratoxin A, citrinin). These mycotoxins often co-occurred naturally in cereals since one kind of crop can be infected by different toxigenic molds and also each mold can produce several kinds of mycotoxins simultaneously. The occurrence of these compounds depends on factors like strain of fungus, species, plant species, and environmental and ecological conditions such as humidity, temperature and presence of pests. This toxicity can range from the production of several hormonal disorders or immunosuppression to the induction of carcinogenic, teratogenic or mutagenic activities. Therefore, the actions of these co-occurring mycotoxins on human or animal can be antagonistic, additive or synergistic.

A Three-Year Survey on the Worldwide Occurrence of Mycotoxins in Feedstuffs and Feed

Between January 2009 and December 2011, a total of 7049 corn, soybean/soybean meal, wheat, dried distillers grains with solubles (DDGS) and finished feed samples were analyzed for the occurrence of aflatoxins (Afla), zearalenone (ZEN), deoxynivalenol (DON), fumonisins (FUM) and ochratoxin A (OTA). Samples were sourced in the Americas, Europe and Asia. Afla, ZEN, DON, FUM and OTA were present respectively in 33%, 45%, 59% 64% and 28% of analyzed samples between 2009 and 2011. From the 23,781 mycotoxin analyzes performed, 81% were positive for at least one mycotoxin. Results of this survey are provided by calendar year, in order to potentially show different trends on mycotoxin occurrence in distinct years: by commodity type and within the same commodity, and by region, to potentially reveal differences in mycotoxin contamination in commodities sourced in diverse regions.