LC-MS/MS multi-method for mycotoxins after single extraction, with validation data for peanut, pistachio, wheat, maize, cornflakes, raisins and figs.

Mycotoxin analysis is usually carried out by high performance liquid chromatography after immunoaffinity column cleanup or in enzyme-linked immunosorbent assay tests. These methods normally involve determination of single compounds only. EU legislation already exists for the aflatoxins, ochratoxin A and patulin in food, and legislation will come into force for deoxynivalenol, zearalenone and the fumonisins in 2007. To enforce the various legal limits, it would be preferable to determine all mycotoxins by routine analysis in different types of matrices in one single extract. This would also be advantageous for HACCP control purposes. For this reason, a multi-method was developed with which 33 mycotoxins in various products could be analysed simultaneously. The mycotoxins were extracted with an acetonitrile/water mixture, diluted with water and then directly injected into a LC-MS/MS system. The mycotoxins were separated by reversed-phase HPLC and detected using an electrospray ionisation interface (ESI) and tandem MS, using MRM in the positive ion mode, to increase specificity for quality control. The following mycotoxins could be analysed in a single 30-min run: Aflatoxins B1, B2, G1 and G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 toxin, HT-2 toxin, alpha-zearalenol, alpha-zearalanol, beta-zearalanol, sterigmatocystin, cyclopiazonic acid, penicillic acid, fumonisins B1, B2 and B3, diacetoxyscirpenol, 3- and 15-acetyl-deoxynivalenol, zearalanone, ergotamin, ergocornin, ergocristin, alpha-ergocryptin, citrinin, roquefortin C, fusarenone X, nivalenol, mycophenolic acid, alternariol and alternariol monomethyl ether. The limit of quantification for the aflatoxins and ochratoxin A was 1.0 microg kg(-1) and for deoxynivalenol 50 microg kg(-1). The quantification limits for the other mycotoxins were in the range 10-200 microg kg(-1). The matrix effect and validation data are presented for between 13 and 24 mycotoxins in peanuts, pistachios, wheat, maize, cornflakes, raisins and figs. The method has been compared with the official EU method for the determination of aflatoxins in food and relevant FAPAS rounds. The multi-mycotoxin method has been proven by the detection of more than one mycotoxin in maize, buckwheat, figs and nuts. The LC-MS/MS technique has also been applied to baby food, which is subject to lower limits for aflatoxin B1 and ochratoxin A, ergot alkaloids in naturally contaminated rye and freeze-dried silage samples.     

LC–MS/MS multi-method for mycotoxins after single extraction,with validation data for peanut,pistachio, wheat,maize, cornflakes,raisins and figs

Mycotoxin analysis is usually carried out by high performance liquid chromatography after immunoaffinity column cleanup or in enzyme-linked immunosorbent assay tests. These methods normally involve determination of single compounds only. EU legislation already exists for the aflatoxins, ochratoxin A and patulin in food, and legislation will come into force for deoxynivalenol, zearalenone and the fumonisins in 2007. To enforce the various legal limits, it would be preferable to determine all mycotoxins by routine analysis in different types of matrices in one single extract. This would also be advantageous for HACCP control purposes. For this reason, a multi-method was developed with which 33 mycotoxins in various products could be analysed simultaneously. The mycotoxins were extracted with an acetonitrile/water mixture, diluted with water and then directly injected into a LC–MS/MS system. The mycotoxins were separated by reversed-phase HPLC and detected using an electrospray ionisation interface (ESI) and tandem MS, using MRM in the positive ion mode, to increase specificity for quality control. The following mycotoxins could be analysed in a single 30-min run: Aflatoxins B₁, B₂, G₁ and G₂, ochratoxin A, deoxynivalenol, zearalenone, T-2 toxin, HT-2 toxin, α-zearalenol, α-zearalanol, β-zearalanol, sterigmatocystin, cyclopiazonic acid, penicillic acid, fumonisins B₁, B₂ and B₃, diacetoxyscirpenol, 3- and 15-acetyl-deoxynivalenol, zearalanone, ergotamin, ergocornin, ergocristin, α-ergocryptin, citrinin, roquefortin C, fusarenone X, nivalenol, mycophenolic acid, alternariol and alternariol monomethyl ether. The limit of quantification for the aflatoxins and ochratoxin A was 1.0 µg kg^?1 and for deoxynivalenol 50 µg kg^?1. The quantification limits for the other mycotoxins were in the range 10–200 µg kg^?1. The matrix effect and validation data are presented for between 13 and 24 mycotoxins in peanuts, pistachios, wheat, maize, cornflakes, raisins and figs. The method has been compared with the official EU method for the determination of aflatoxins in food and relevant FAPAS rounds. The multi-mycotoxin method has been proven by the detection of more than one mycotoxin in maize, buckwheat, figs and nuts. The LC–MS/MS technique has also been applied to baby food, which is subject to lower limits for aflatoxin B₁ and ochratoxin A, ergot alkaloids in naturally contaminated rye and freeze-dried silage samples.     

Mycotoxin contamination of sorghum and its contribution to human dietary exposure in four sub-Saharan countries

This research aimed at evaluating the safety, and the type, level and prevalence of mycotoxins in grain sorghum of four sub-Saharan African (SSA) countries (Burkina Faso, Ethiopia, Mali and Sudan). A multi-analyte LC-MS/MS method for quantification of 23 mycotoxins (nivalenol, deoxynivalenol, fusarenon X, neosolaniol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, diacetoxyscirpenol, roquefortine C, HT-2 toxin, alternariol, T-2 toxin, FB1, FB2, FB3, zearalenone, aflatoxin G₁, aflatoxin G₂, aflatoxin B₁, aflatoxin B₂, sterigmatocystin, OTA, altenuene, alternariol monomethylether) was applied to different sorghum matrices. Of the 1533 analysed samples, 33% were contaminated with at least one of the following mycotoxins: aflatoxins, fumonisins, sterigmatocystin, Alternaria toxins, OTA and zearalenone. Country of origin, colour, source and collection period of sorghum samples significantly influenced the type, level and prevalence of mycotoxins. Sterigmatocystin (15%), fumonisins (17%) and aflatoxins (13%) were the most prevalent. FB1 (274 ± 585 µg/kg) had the highest mean concentration followed by FB2 (214 ± 308 µg/kg) while diacetoxyscirpenol (8.12 ± 19.2 µg/kg) and HT-2 (11.9 ± 0.00 µg/kg) had the lowest concentrations. Neosolaniol, fusarenon-X, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, T-2 toxin, nivalenol and roquefortine C were not detected in any of the samples. Sudan had the lowest prevalence and mean concentration of all mycotoxins. Pink sorghum had the highest concentrations of fumonisins and aflatoxins. Mycotoxins from Aspergillus spp. and Alternaria spp. are the mycotoxins of concern in SSA grain sorghum with regard to prevalence, concentration and possible health risk from exposure. Based on the performed risk characterisation, daily consumption of sorghum containing aflatoxins, alternariol, alternariol monomethyl ether, sterigmatocystin and OTA could result in exceeding the established health-based guidance values for these toxins.     

Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra-high performance liquid chromatography/tandem mass spectrometry

A rapid, reliable and sensitive method was developed to determine 12 mycotoxins (deoxynivalenol, aflatoxins B1, B2, G1, G2 and M1, fumonisins B1 and B2, ochratoxin A, HT-2 and T-2 toxin and zearalenone) simultaneously in maize, walnuts, biscuits and breakfast cereals. The method is based on a single extraction step using acetonitrile/water mixture (80/20 v/v) followed by ultra-high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The selectivity of the MS/MS detection allowed the elimination of further clean up steps. Extraction, chromatographic and detection conditions were optimised in order to increase sample throughput and sensitivity. Matrix-matched calibration was used for quantification and recoveries of the extraction process ranged from 70.0% and 108.4%, with relative standard deviations lower than 25% in all the cases, when samples were fortified at 5 and 50 μg/kg. Limits of detection ranged from 0.01 to 2.1 μg/kg and limits of quantification ranged from 0.03 to 6.30 μg/kg, which were always below the tolerance levels of mycotoxins set by European Union in the matrices evaluated. Several samples were analysed and aflatoxins B1, B2, G1, G2 and T-2 toxin were detected in one maize sample, with concentrations lower than 6.0 μg/kg and deoxynivalenol was detected in a breakfast cereal at 42.1 μg/kg.     

Stability of mycotoxins during food processing

The mycotoxins that commonly occur in cereal grains and other products are not completely destroyed during food processing operations and can contaminate finished processed foods. The mycotoxins most commonly associated with cereal grains are aflatoxins, ochratoxin A, fumonisins, deoxynivalenol and zearalenone. The various food processes that may have effects on mycotoxins include sorting, trimming, cleaning, milling, brewing, cooking, baking, frying, roasting, canning, flaking, alkaline cooking, nixtamalization, and extrusion. Most of the food processes have variable effects on mycotoxins, with those that utilize the highest temperatures having greatest effects. In general the processes reduce mycotoxin concentrations significantly, but do not eliminate them completely. However, roasting and extrusion processing show promise for lowering mycotoxin concentrations, though very high temperatures are needed to bring about much of a reduction in mycotoxin concentrations. Extrusion processing at temperatures greater than 150 degrees C are needed to give good reduction of zearalenone, moderate reduction of alfatoxins, variable to low reduction of deoxynivalenol and good reduction of fumonisins. The greatest reductions of fumonisins occur at extrusion temperatures of 160 degrees C or higher and in the presence of glucose. Extrusion of fumonisin contaminated corn grits with 10% added glucose resulted in 75-85% reduction in Fumonisin B(1) levels. Some fumonisin degredation products are formed during extrusion, including small amounts of hydrolyzed Fumonisin B(1) and N-(Carboxymethyl) - Fumonisin B(1) and somewhat higher amounts of N-(1-deoxy-d-fructos-1-yl) Fumonisin B(1) in extruded grits containing added glucose. Feeding trial toxicity tests in rats with extruded fumonisin contaminated corn grits show some reduction in toxicity of grits extruded with glucose.     

粮油食品中真菌毒素的LC-MS法检测

粮油食品中常见的真菌毒素有:黄曲霉毒素、赭(棕)曲霉毒素、展青霉毒素、玉米赤霉烯酮、串珠镰刀菌毒素及脱氧雪腐镰刀菌烯醇等,因含量较低,用常规方法检测不出来。用LC-MS检测,灵敏度高、前处理比较简单,结果准确可靠,在检测食品中真菌毒素上前景广阔。     

Survey for aflatoxins, ochratoxin A, zearalenone and fumonisins in maize imported into the United Kingdom

This survey examined 140 samples of raw maize as received at ports or at major maize mills in the UK and 12 after initial cleaning. Samples were examined for aflatoxins B₁, B₂, G₁ and G₂, ochratoxin A, zearalenone and fumonisins B₁, B₂ and B₃ using fully validated analytical HPL C methods with detection limits of 0.1 mu g/kg for each aflatoxin and ochratoxin A, 4 mu g/ kg for zearalenone and 10 mu g/kg for each fumonisin. 95.0% and 92.1% of samples met the new EC statutory maximum permissible level for total aflatoxins and aflatoxin B₁ respectively. The maximum concentration of ochratoxin A found was 1.5 mu g/kg. Zearalenone and fumonisins were detected in almost every sample with 41.7% of maize containing more than 100 mu g/kg of zearalenone and 48% of samples containing more than 1000 mu g/kg total fumonisins. Initial cleaning of raw maize reduced aflatoxin concentrations by about 40% and total fumonisins by 32%.     

Mycotoxins in infant/toddler foods and breakfast cereals in the US retail market

The objective of this study was to conduct a mycotoxin survey of commercial infant/toddler foods (cereals and teething biscuits) and breakfast cereals in the United States. A total of 215 retail samples were collected from three geographical locations and analysed for aflatoxins, fumonisins, deoxynivalenol, HT-2 toxin, ochratoxin A, T-2 toxin, and zearalenone using a stable isotope dilution liquid-chromatography tandem mass spectrometry (LC-MS/MS) method. One or more mycotoxins were found in 69% (101/147) of the infant/toddler foods and 50% (34/68) of breakfast cereals. Mycotoxin co-occurrence was observed in 12% of infant/toddler foods and 32% of breakfast cereals. However, the concentrations of detected mycotoxins were lower than the current FDA action and guidance levels. Aflatoxins and HT-2 toxin were not detected in any of the samples, while deoxynivalenol was the most frequently detected mycotoxin. Rice-based cereals appeared to be less susceptible to mycotoxin contamination than other cereal types.     

Evaluation of LC-high-resolution FT-Orbitrap MS for the quantification of selected mycotoxins and the simultaneous screening of fungal metabolites in food

A liquid chromatography-high-resolution mass spectrometry-based method is reported for the quantification of 20 selected mycotoxins and the simultaneous screening for 200 fungal metabolites in food. For regulated mycotoxins, such as aflatoxins, fumonisins, ochratoxin A, zearalenone and trichothecenes, the evaluation of the method performance characteristics, such as precision, trueness, limit of detection and matrix effects, has been exemplified for the matrix maize. In the case of the limit of detection, an alternative evaluation approach for high-resolution FT-Orbitrap data is proposed. Measurements of the signal-to-noise ratios obtained from 'full-profile mode' data led to detection limits between 8 and 160?ng?g(-1). Eight naturally contaminated wheat- and maize-based matrix test materials, originating from interlaboratory comparison studies, were used to confirm the trueness of the method for deoxynivalenol, zearalenone, fumonisin B(1) and B(2), HT-2, and T-2 toxin. In addition to accurate quantification of the most relevant mycotoxins, the full-scan chromatograms were used to investigate the potential of the FT-Orbitrap to screen simultaneously for a large number of fungal metabolites. First, a list of 200 metabolites, potentially being present in food samples, was established. Next, specific detection and identification criteria were defined, which are based on accurate mass, peak intensity and isotopologue ratio. The application of these criteria to the suspected metabolites from the list resulted in the putative identification of 13 fungal metabolites in addition to the target toxins.     

The Fate of Mycotoxins During the Processing of Wheat for Human Consumption

Mycotoxins are a potential health threat in cereals including wheat. In the European Union (EU), mycotoxin maximum levels are laid down for cereal raw materials and final food products. For wheat and wheat‐based products, the EU maximum levels apply to deoxynivalenol (DON), zearalenone, aflatoxins, and ochratoxin A. This review provides a comprehensive overview on the different mycotoxins and their legal limits and on how processing of wheat can affect such contaminants, from raw material to highly processed final products, based on relevant scientific studies published in the literature. The potential compliance with EU maximum levels is discussed. Of the four mycotoxins regulated in wheat‐based foods in the EU, most data are available for DON, whereas aflatoxins were rarely studied in the processing of wheat. Furthermore, available data on the effect of processing are outlined for mycotoxins not regulated by EU law—including modified and emerging mycotoxins—and which cover DON derivatives (DON‐3‐glucoside, mono‐acetyl‐DONs, norDONs, deepoxy‐DON), nivalenol, T‐2 and HT‐2 toxins, enniatins, beauvericin, moniliformin, and fumonisins. The processing steps addressed in this review cover primary processing (premilling and milling operations) and secondary processing procedures (such as fermentation and thermal treatments). A special focus is on the production of baked goods, and processing factors for DON in wheat bread production were estimated. For wheat milling products derived from the endosperm and for white bread, compliance with legal requirements seems to be mostly achievable when applying good practices. In the case of wholemeal products, bran‐enriched products, or high‐cereal low‐moisture bakery products, this appears to be challenging and improved technology and/or selection of high‐quality raw materials would be required.     

A survey of fumonisins, deoxynivalenol, zearalenone and aflatoxins contamination in corn-based food products in Argentina.

The presence of mycotoxins in corn-based foods available in Argentina was determined in order to make a preliminary exposure assessment. Thirty-eight samples [corn meal ('polenta') and corn flakes] of different local brands were analysed for zearalenone, deoxynivalenol and aflatoxins by TLC and fumonisins (FB1, FB2 and FB3) by HPLC. None of the 38 samples contained any detectable amount of aflatoxins (< 2 micrograms/kg), zearalenone (< 50 micrograms/kg) and deoxynivalenol (< 50 micrograms/kg). By contrast fumonisin contamination was found in 95% of the samples. The highest fumonisin levels were found in corn meal: FB1 (range positives: 60-2860 micrograms/kg; mean positive value: 556 micrograms/kg), FB2 (61-1090 micrograms/kg; 232 micrograms/kg) and FB3 (18-1015 micrograms/kg; 150 micrograms/kg). Low levels of fumonisin B1 were detected in 16/17 corn flakes samples (2-38 micrograms/kg). Total fumonisin levels in corn meal were more than 1000 micrograms/kg in 24% (5/21) of the samples. Although it is not the staple food in Argentina, maize consumption is very important, especially among children. A daily fumonisin intake of 11.3 micrograms/kg of body weight was estimated for child consumers (1-5 years old) based on an average consumption of 200 g of corn meal/day. Calculated at an average rate for all children (consumers or not) the intake estimate was 0.9 microgram/kg of body weight.     

Co-occurrence of mycotoxins in commercial formula milk and cereal-based baby food on the Qatar market

The present study was conducted to explore the occurrence of mycotoxins in commercial baby foods in Doha-Qatar. LCMS/MS- and HPLC-based analysis of baby food (n = 67) for 12 mycotoxins confirmed the presence of aflatoxin M1 (AFM1, 33%), ochratoxin A (OTA, 31%), deoxynivalenol (DON, 27%), aflatoxin B1 (AFB1, 22%), fumonisin B2 (FB2, 10%), zearalenone (ZEN, 4%) and T-2 toxin (2%). Noodles exhibited the maximum contamination percentage, with 33% of the samples being contaminated above the EU maximum limits, for at least one mycotoxin. Among the multi-grain flake samples, up to 28% and for the milk and milk-based-cereal samples, 14% contained at least one mycotoxin above the EU maximum limits. From all cereal-based food samples, 22%, 5%, 2% and 2% were concurrently contaminated with 2, 3, 4 and 5 mycotoxins, respectively. The occurrence of toxicological important mycotoxins in Qatari market warrants the implementation of strict regulatory limits to protect human health.     

Mycotoxins in corn and wheat silage in Israel

Silage is an important feed source for intensive dairy herds worldwide. Fungal growth and mycotoxin production before and during silage storage is a well-known phenomenon, resulting in reduced nutritional value and a possible risk factor for animal health. With this in mind, a survey was conducted to determine for the first time the occurrence of mycotoxins in corn and wheat silage in Israel. A total of 30 corn and wheat silage samples were collected from many sources and analysed using a multi-mycotoxin method based on LC-MS/MS. Most mycotoxins recorded in the present study have not been reported before in Israel. Overall, 23 mycotoxins were found in corn silage; while wheat silage showed a similar pattern of mycotoxin occurrence comprising 20 mycotoxins. The most common post-harvest mycotoxins produced by the Penicillium roqueforti complex were not found in any tested samples, indicative of high-quality preparation and use of silage. Moreover, none of the European Union-regulated mycotoxins – aflatoxin B1, ochratoxin, T-2 toxin, diacetoxyscirpenol and deoxynivalenol – were found above their limits of detection (LODs). The Alternaria mycotoxins – macrosporin, tentoxin and alternariol methyl ether – were highly prevalent in both corn and wheat silage (>80%), but at low concentrations. The most prominent (>80%) Fusarium mycotoxins in corn silage were fusaric acid, fumonisins, beauvericin, monilifomin, equisetin, zearalenone and enniatins, whereas in wheat silage only beauvericin, zearalenone and enniatins occurred in more than 80% of the samples. The high prevalence and concentration of fusaric acid (mean = 765 µg kg^–1) in Israeli corn silage indicates that this may be the toxin of highest potential concern to dairy cow performance. However, more data from different harvest years and seasons are needed in order to establish a more precise evaluation of the mycotoxin burden in Israeli silage.     

Determination of aflatoxins,deoxynivalenol, ochratoxin A and zearalenone in organic wheat flour under different storage conditions

Samples of flour derived from an organic wheat seed cultivated in the region Abruzzo (Central Italy) were examined for the detection of aflatoxins, deoxynivalenol, ochratoxin A and zearalenone after storage in the presence of oxygen or under vacuum, for one year. They were analysed by high-performance liquid chromatography with fluorescence detection for aflatoxins, ochratoxin A and zearalenone and with diode array detector for deoxynivalenol. An immunoaffinity column clean-up was applied for all the compounds, except for aflatoxin determination, which required a solid-phase extraction. Recoveries (range: 76–107%) and within-laboratory reproducibility (RSD% < 10.3) met the performance criteria of Commission Regulation (EU) No. 519/2014 amending Commission Regulation (EC) No. 401/2006 for the detection of mycotoxins in foodstuffs. Analytes were below the detection limit of the method, and this result was probably due to the quality of organic seed and good agricultural practices performed for the prevention of mycotoxin formation.     

The fate of mycotoxins during secondary food processing of maize for human consumption

Mycotoxins are naturally occurring fungal metabolites that are associated with health hazards and are widespread in cereals including maize. The most common mycotoxins in maize that occur at relatively high levels are fumonisins (FBs), zearalenone, and aflatoxins; furthermore, other mycotoxins such as deoxynivalenol and ochratoxin A are frequently present in maize. For these toxins, maximum levels are laid down in the European Union (EU) for maize raw materials and maize-based foods. The current review article gives a comprehensive overview on the different mycotoxins (including mycotoxins not regulated by EU law) and their fate during secondary processing of maize, based on the data published in the scientific literature. Furthermore, potential compliance with the EU maximum levels is discussed where appropriate. In general, secondary processing can impact mycotoxins in various ways. Besides changes in mycotoxin levels due to fractionation, dilution, and/or concentration, mycotoxins can be affected in their chemical structure (causing degradation or modification) or be released from or bound to matrix components. In the current review, a special focus is set on the effect on mycotoxins caused by different heat treatments, namely, baking, roasting, frying, (pressure) cooking, and extrusion cooking. Production processes involving multiple heat treatments are exemplified with the cornflakes production. For that, potential compliance with FB maximum levels was assessed. Moreover, effects of fermentation of maize matrices and production of maize germ oil are covered by this review.     

高效液相色谱-串联质谱法测定杂粮豆类中11种真菌毒素

利用高效液相色谱-串联质谱建立杂粮豆类中11种真菌毒素（包括黄曲霉毒素B1、B2、G1、G2、赭曲霉毒素A、T-2毒素、脱氧雪腐镰刀菌烯醇、伏马毒素B1、B2和B3、玉米赤霉烯酮）同时检测的方法。实验对提取溶剂、提取时间和净化方式等进行优化,建立双体系联合提取方法,首先采用甲醇-水（70∶30,V/V）体系提取,再以乙腈-水（84∶16,V/V）体系二次提取,提取时间3 min,在此基础上采用C18吸附剂进行净化处理。结果表明,11种毒素的线性范围良好,相关系数大于0.999,添加回收率为70.0%～108%,相对标准偏差为1.3%～8.6%。所建方法简单、快速、灵敏度高、重复性好,可满足杂粮豆类中11 种真菌毒素的同时检测需要。     

Quantitative analysis of mycotoxins in cereal foods by collision cell fragmentation-high-resolution mass spectrometry: performance and comparison with triple-stage quadrupole detection

A liquid chromatography-high-resolution mass spectrometry (LC-HRMS) method for the simultaneous determination of aflatoxins (B(1), B(2), G(1), G(2)), ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2 toxins in wheat flour, barley flour and crisp bread was developed. Mycotoxin fragmentation patterns obtained by high-energy collision dissociation (HCD) were investigated to obtain quantitative and confirmatory information (two characteristic masses per mycotoxin) using Orbitrap?-based high-resolution mass spectrometry. LC-HRMS (full-scan) detection carried out by HCD allows the monitoring of the pseudo-molecular ion and an additional characteristic fragment (for each mycotoxin) with mass accuracy in the range 0.1-3.9?ppm, meeting current European regulatory requirements for LC-MS confirmatory analysis. A sample preparation procedure based on polymeric solid-phase extraction cartridges was applied, allowing recoveries higher than 74% for nine mycotoxins, with a relative standard deviation lower than 13%. Detection limits in the range 0.5-3.4?μg?kg(-1) were obtained for three cereal matrices. A critical comparison between the proposed method and a validated method based on triple quadrupole mass spectrometry showed similar performance in terms of detection limits, recoveries and repeatability, and matrix effects. Based on an efficient sample extraction and clean-up, the LC-HCD-HRMS method reported here represents a reliable and robust alternative tool for mycotoxin analysis in food matrices as compared with well-established triple quadrupole-based approaches.     

Multimycotoxin Determination in Tunisian Farm Animal Feed

Mycotoxins presence was evaluated in animal feed marketed in Tunisia for the first time ever. A QuEChERS method was performed to analyze the natural copresence of 22 mycotoxins (enniatins, beauvericin, ochratoxin A, aflatoxins, alternariol monomethyl ether, alternariol, tentoxin, zearalenone, deoxynivalenol, 3‐acetyldeoxynivalenol, 15‐acetyldeoxynivalenol, nivalenol, neosolaniol, diacetoxyscirpenol, T‐2 toxin, and HT‐2 toxin) in 122 Tunisian marketed feed samples, intended for poultry (n = 43), cattle (n = 35), rabbit (n = 12), sheep (n = 16), and horse (n = 16). Analytes detection and quantification were done using both liquid chromatography and gas chromatography coupled to tandem mass spectrometry. The analytical method showed good linearity (R > 0.996) and sensitivity, the limits of quantification ranged from 0.1 ng/g (enniatin A1) to 225 ng/g (3‐acetyldeoxynivalenol). Eighty‐five percent of the analyzed samples were positive. Poultry (n = 43) and rabbit (n = 12) feed samples were the most contaminated. Enniatin B was the most prevalent mycotoxin with values ranged between 0.5 ng/g for horse feed and 40 ng/g for poultry feed, followed by deoxynivalenol detected from 16 ng/g in cattle feed to 250 ng/g in poultry feed. None exceeded the limits set by EU recommendations for animal feed. Mycotoxins co‐occurrence was observed at most by five different mycotoxins (26%) and up to eight mycotoxins was recorded in 5% of samples. Furthermore, a relatively high copresence rate of different fusariotoxins was registered. Even if no toxicological concern was clearly revealed, the contamination is a real fact and will probably present influence on meat production and on food safety.     

Mycotoxins in infant cereal foods from the Canadian retail market

Three hundred and sixty-three samples of cereal-based infant foods were collected from the Canadian retail marketplace over 3 years. The samples included oat-, barley-, soy-, and rice-based infant cereals, mixed-grain infant cereals, teething biscuits, creamed corn, and soy-based formulas. Samples were analysed for targeted mycotoxins (deoxynivalenol, nivalenol, HT-2 toxin, zearalenone, ochratoxin A, fumonisins B₁ and B₂, and five ergot alkaloids). Soy-based cereals (which usually contain corn) exhibited the highest incidences of deoxynivalenol (100%), zearalenone (46%) and fumonisins (75%). Overall, deoxynivalenol was the most frequently detected mycotoxin -- it was detected in 63% of samples analysed. Survey results demonstrated the regular occurrence of multiple mycotoxins in cereal-based infant foods.     

Application of hybrid linear ion trap-high resolution mass spectrometry to the analysis of mycotoxins in beer

This paper reports the application of liquid chromatography electrospray ionization ion trap-orbitrap mass spectrometry for the determination of 18 mycotoxins (aflatoxins, fumonisins, trichothecenes, ochratoxin A, sterogmatocystin, beauvaricin, zearalenone and zearalenol) in beer. The extraction procedure was carried out by solid phase extraction (SPE): SPE columns were conditioned with acetonitrile/methanol and water. Beer was loaded onto the column which was washed with water. In these conditions, the recoveries were more than 65% and the relative standard deviation (RSD) were below 18%. The lowest limits of quantification (LLOQ) ranged from 9 to 155?ng?ml(-1). Matrix-matched calibration was performed for each beer and reliable results were obtained from selected mycotoxins. The method was applied to the analysis of 25 commercial beers. Taking advantage of the hybrid capabilities, the presence of other mycotoxins were checked; enniatins (A, A(1), B and B(1)) and fusaproliferin were studied in all the tested samples. The survey detected the presence of zearalenone in one stout beer sample.