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Beltrami D.,University of Parma | Calestani D.,CNR Institute of Materials for Electronics and Magnetism | Maffini M.,University of Parma | Suman M.,Barilla Food Research Labs | And 6 more authors.
Analytical and Bioanalytical Chemistry | Year: 2011

An integrated approach based on the use of inductively coupled plasma mass spectrometry (ICP-MS) and scanning electron microscopy (SEM) for the qualitative and quantitative analyses of metal particles in foods was devised and validated. Different raw materials and food products, like wheat, durum wheat, wheat flour, semolina, cookies, and pasta were considered. Attention was paid to the development of sample treatment protocols for each type of sample to avoid potential artifacts such as aggregation or agglomeration. The analytical protocols developed followed by ICP-MS and SEM investigations allowed us the quantitative determination and the morphological and dimensional characterization of metal nano- and microparticles isolated from the raw materials and finished food products considered. The ICP-MS method was validated in terms of linearity (0.8-80 μg/g and 0.09-9 μg/g for Fe and Ti, respectively), quantification limits (0.73 μg/g for Fe and 0.09 μg/g for Ti), repeatability (relative standard deviation (RSD) % equal to 10% for Fe and 20% in a wheat matrix as an example), and extraction recoveries (93∈±∈2-101∈±∈2%). Validation of the scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) measurements was performed working in a dimensional range from 1 to 100 μm with an estimated error in the size determination equal to 0.5 μm. ICP-MS data as well as SEM measurements showed a decrease in the concentration of metal particles from wheat to flour and from durum wheat to semolina samples, thus indicating an external contamination of grains by metal particles. These findings were confirmed by environmental SEM analysis, which allowed investigation of particles of lower dimensions. Generally, the largest number of particles was found in the case of iron and titanium, whereas particles of copper and zinc were only occasionally found without any possibility of quantifying their number. © 2011 Springer-Verlag.


Valenzano S.,CNR Institute of Sciences of Food Production | Lippolis V.,CNR Institute of Sciences of Food Production | Pascale M.,CNR Institute of Sciences of Food Production | De Marco A.,CNR Institute of Sciences of Food Production | And 3 more authors.
Food Analytical Methods | Year: 2014

A rapid and accurate fluorescence polarization (FP) immunoassay has been optimized for the determination of deoxynivalenol (DON) in wheat bran and whole-wheat flour. A preliminary treatment with activated charcoal was used to eliminate the strong matrix effect due to highly colored interfering compounds present in raw wheat bran extracts. In particular, matrix effect was removed by adding activated charcoal to the wheat bran extract (3.5 mg/mL) and mixing for 3 min of incubation time prior to the FP immunoassay analysis. No preliminary treatment was necessary for whole-wheat flour. Average recoveries from samples spiked with DON at levels of 500, 1,000, and 1,500 μg/kg were 95 % for wheat bran and 94 % for whole-wheat flour, with relative standard deviation generally lower than 13 %. Limits of quantification of the optimized FP immunoassay were 120 μg/kg for both matrices. The overall time of analysis was lower than 15 min for wheat bran and 10 min for whole-wheat flour. Good correlations (r > 0.971) were observed between DON contents obtained by both FP immunoassay and high-performance liquid chromatography with immunoaffinity cleanup for 37 and 23 samples of naturally contaminated wheat bran and whole-wheat flour, respectively. These results show that the FP immunoassay is suitable for high-throughput screening as well as for quantitative determination of DON in wheat bran and whole-wheat flour. © 2013 Springer Science+Business Media New York.


Porricelli A.C.R.,CNR Institute of Sciences of Food Production | Lippolis V.,CNR Institute of Sciences of Food Production | Valenzano S.,CNR Institute of Sciences of Food Production | Cortese M.,CNR Institute of Sciences of Food Production | And 3 more authors.
Food Analytical Methods | Year: 2016

A fluorescence polarization (FP) immunoassay has been optimized and validated for rapid quantification of T-2 and HT-2 toxins in both unprocessed cereals, including oats, barley and rye, and cereal-based products for direct human consumption, such as oat flakes, oats crispbread and pasta. Samples were extracted with 90 % methanol, and the extract was filtered and diluted with water or sodium chloride solution prior to the FP immunoassay. Overall mean recoveries from spiked oats, rye, barley, oat flakes, oats crispbread and pasta ranged from 101 to 107 %, with relative standard deviations lower than 7 %. Limits of detection (LODs) of the FP immunoassay were 70 μg/kg for oats, 40 μg/kg for oat flakes and barley, 25 μg/kg for pasta and 20 μg/kg for rye and oats crispbread. The trueness of the immunoassay was assessed by using two oat and oat flake reference materials for T-2 and HT-2 toxins, showing good accuracy and precision. Good correlations (r > 0.953) were observed between T-2 and HT-2 toxin contents in naturally and artificially contaminated samples determined by both FP immunoassay and ultra-high-performance liquid chromatography (UHPLC) with immunoaffinity column cleanup used as reference method. These results, combined with rapidity and simplicity of the assay, show that the optimized assay is suitable for high-throughput screening, as well as for reliable quantitative determination of T-2 and HT-2 toxins in cereals and cereal-based products. © 2016 Springer Science+Business Media New York


Lippolis V.,CNR Institute of Sciences of Food Production | Pascale M.,CNR Institute of Sciences of Food Production | Valenzano S.,CNR Institute of Sciences of Food Production | Porricelli A.C.R.,CNR Institute of Sciences of Food Production | And 2 more authors.
Food Analytical Methods | Year: 2014

A sensitive and accurate fluorescence polarization (FP) immunoassay has been developed for the determination of ochratoxin A (OTA) in naturally contaminated wheat samples. A fluorescein-labeled OTA tracer was synthesized, and its binding response with three monoclonal antibodies was tested. The most sensitive competitive FP immunoassay showed an IC50 value of 0.48 ng/mL with a negligible cross-reactivity for ochratoxin B (1.7 %) and no cross-reactivity with other mycotoxins commonly occurring in wheat. The wheat sample was extracted with acetonitrile/water (60:40, v/v) and purified by a rapid solid-phase extraction procedure using an aminopropyl column prior to the FP immunoassay. The overall time of analysis was less than 20 min. The average recovery from spiked wheat samples (3 to 10 μg/kg) was 87 %, with relative standard deviations generally lower than 6 %. Limits of detection and quantification were 0.8 and 2.0 μg/kg, respectively. The trueness of the method was assessed by using two reference materials for OTA showing good accuracy and precision. A good correlation (r = 0.995) was observed between OTA contamination of 19 naturally contaminated wheat samples analyzed by both FP immunoassay and high-performance liquid chromatography/immunoaffinity clean-up used as reference method. These results show that the developed FP method is suitable for high-throughput screening, as well as for reliable quantitative determination of OTA in wheat at level far below the EU regulatory limits. © 2013 Springer Science+Business Media New York.


Bergamini E.,Barilla Food Research Labs | Catellani D.,Barilla Food Research Labs | Dall'asta C.,University of Parma | Galaverna G.,Barilla Food Research Labs | And 3 more authors.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2010

Fusarium mycotoxins are a relevant problem in the cereal supply chain at a worldwide level, with wheat, maize and barley being the main contaminated crops. Mould growth can happen in the pre-harvest phase and also during transport and storage due to ineffective drying conditions. Among Fusarium toxins, deoxynivalenol (DON) is considered the most important contaminant in wheat due to its widespread occurrence. In the last years the European Food Safety Authority (EFSA) and the European Commission have frequently expressed opinions on Fusarium toxins, setting limits, regulations and guidelines in order to reduce their levels in raw materials and food commodities. In particular, European legislation (Reg. 1881/2006) sets the maximum limit for DON in flour and bread as 750 and 500 μgkg-1 respectively. Relatively few studies have taken into account the loss of trichothecenes during processing, focusing on how processing factors may influence their degradation. In particular, the description of DON behaviour during bread-making is very difficult, since complex physico-chemical modifications occur during the transformation of the raw ingredients into the final product. In the present study, we studied how DON concentration may be influenced by modifying bread-making parameters, with a special emphasis on the fermentation and baking stages, starting from a naturally contaminated flour at both pilot and industrial scales. Exploiting the power of a Design of Experiments (DoE) approach to consider the great complexity of the studied system, the obtained model shows satisfying goodness-of-fit and prediction, suggesting that the baking step (time/temperature ranges) is crucial for minimizing native DON level in bread. © 2010 Taylor & Francis.


Suman M.,Barilla Food Research Labs | Manzitti A.,Barilla Food Research Labs | Catellani D.,Barilla Food Research Labs
World Mycotoxin Journal | Year: 2012

Fusarium mycotoxins represent a significant problem in the cereal supply chain, with wheat, maize and barley being the main contaminated crops. Among the Fusarium toxins, the trichothecene deoxynivalenol (DON) is considered to be the most important contaminant in wheat due to its widespread occurrence. To protect consumers from unacceptably high trichothecene intakes in their diets, many countries have set maximum trichothecene levels for cereals and related food commodities. Relatively few studies have considered the loss of trichothecenes during industrial processing and focused on how processing steps may influence their degradation or modification. The aim of the present study is to verify how the DON and deoxynivalenol-3-glucoside (DON-3G) concentration in wholegrain crackers can be influenced by changes to the technological parameters employed during the fermentation and baking steps, starting with naturally contaminated bran, using a pilot-scale plant and exploiting the power of the Design of Experiments (DoE) approach. The DON results were then used to generate a preliminary predictive model, suggesting that the baking step represents the most important phase in minimising the native toxin level in crackers. © 2012 Wageningen Academic Publishers.


Mattarozzi M.,University of Parma | Lambertini F.,Barilla Food Research Labs | Suman M.,Barilla Food Research Labs | Careri M.,University of Parma
Journal of Chromatography A | Year: 2013

European Union legislation has established that plastic food contact materials shall not release primary aromatic amines (PAAs), which are toxic compounds and suspected human carcinogens. As valid alternative to existing methods for PAA determination, which are based on spectrophotometric test or targeted liquid chromatography-tandem mass spectrometry (LC-MS/MS) approaches, in this study a LC-Orbitrap-full scan-high resolution mass spectrometry (HRMS) method was devised and validated for the determination of migration levels of 22 PAAs from food contact materials, thus exploiting the specificity of accurate mass measurement. Direct injection of the simulant (acetic acid 3%, w/v) into the LC-MS system after migration, without any pre-treatment step, makes the developed method of great value for rapid screening analysis of a large number of amines. A very fast and efficient separation (<11min) of PAAs was achieved. Detection limits in the 0.06-0.7μgkg-1 range were calculated for 17 out of 22 of the investigated PAAs, however obtaining values within 5.3μgkg-1 for the other 5 amines. Good dynamic linear ranges from two to four orders of magnitude (r2≥0.990) were obtained and satisfying results were achieved in terms of intra-day (RSDs<10%) and inter-day repeatability (RSDs<17%). Trueness values in the 70±1-131±5% range proved reliability of the developed method for PAAs quantification also at very low concentration levels. Finally, the method was successfully applied to a range of different real plastic multilayer food packaging materials, noticing in all cases levels below the established limits of detection. © 2013 Elsevier B.V.


Primary aromatic amines (PAAs) can migrate from packaging into food from different sources such as polyurethanic adhesives used for the manufacture of multilayer films, which may contain residual aromatic isocyanates, or recycled paperboard, because of the presence of azo dyes in the printed paper massively used in the recycling process. In the present work, a reliable analytical method, exploiting a conventional high-performance liquid chromatography-(selected ion monitoring)-mass spectrometry system, for PAAs compliance assessment in food contact materials was developed as an effective alternative to the current standard spectrophotometric one, moving in this way from the screening to the accurate and selective quantitation perspective for the analysis of PAAs both in aqueous and acidic food simulants. The main validation parameters were verified achieving very satisfactory results in terms of linearity range, limit of detection (ranging from 0.1 to 1.0gkg(-1)) and quantitation (ranging from 0.1 to 3.6gkg(-1)), repeatability and accuracy. Suitability of the method was demonstrated for a wide range of commercial samples, chosen among different producers of the most common used food packaging plastic and paperboard categories and then analyzed to assess the risk related to PAAs migration. Finally, the method was also successfully exploited to monitor the evolution of potential PAAs migration during the industrial curing process of multilayer plastic laminates, prior to their release for delivery to the food industry end user.

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