Ochratoxin A and Sterigmatocystin in Long-Ripened Grana Cheese: Occurrence, Wheel Rind Contamination and Effectiveness of Cleaning Techniques on Grated Products.

A survey on the occurrence of ochratoxin A (OTA) and sterigmatocystin (STC) in grated cheese products obtained from hard grana-type cheeses was carried out, where 107 grated products were collected in retail outlets and analysed. OTA and STC were found in 48.6% and 94.4% of the samples, in a range from

Acrylamide determination during an industrial roasting process of coffee and the influence of asparagine and low molecular weight sugars.

The formation and partial degradation of acrylamide (AA), asparagine and low molecular weight sugars were evaluated during an industrial coffee roasting process, in which the temperature increased from 90° to about 215 °C. Arabica and Robusta varieties were roasted individually. AA content reached the maximum value at 10 min, corresponding to a temperature of 175-177 °C (1045 ±â€¯28 and 795 ±â€¯25 µg kg-1 for Arabica and Robusta, respectively). Successively, AA content decreased very quickly and at 14 min (203-205 °C) its concentration was lower than the benchmark level of 400 µg kg-1 for roast coffee set by the EU Commission Regulation (2017/2158). In the final product, AA content was close to 300 µg kg-1. Asparagine quickly decreased; contrary, the concentration of fructose and glucose increased reaching their maximum value at 12 min. Then, a quick degradation occurred; their increase could be mainly due to the hydrolysis of sucrose, which decreased in the same period.

LC-MS/MS and LC-UV Determination of Moniliformin by Adding Lanthanide Ions to the Mobile Phase.

An innovative chromatographic analysis was developed for the determination of moniliformin (MON). Because of its ionic nature, MON is weakly retained in reversed-phase chromatography and the separation may be tricky. Nevertheless, this technique is normally used either with the formation of ion pairs or employing specific RP columns for polar compounds, or combining anion exchange and hydrophobic interactions. Hydrophilic interaction chromatography (HILIC) was also used, but a non-negligible peak tailing was observed. Besides its ionic nature, MON is a di-ketone and di-ketones, mainly ß-di-ketones, can easily form complexes with lanthanide ions. Then, in this work the addition of lanthanide ions to the mobile phase was investigated, aiming at improving peak shape and MON separation. La3+, Tb3+ or Eu3+ aqueous solutions were used as mobile phase and MON was chromatographed using a LC-NH2 column. The probable formation of coordination complexes lanthanide-MON in the HPLC mobile phase allowed to obtain a symmetrical peak shape and a satisfactory chromatographic separation by both mass spectrometry (MS/MS) and UV detection. Finally, a suitable extraction and purification method for MON determination in cereal samples was developed.

Efficacy of Azoxystrobin on Mycotoxins and Related Fungi in Italian Paddy Rice.

The efficacy of azoxystrobin was evaluated in the presence of mycotoxigenic fungi and relative mycotoxins in Italian paddy rice during the growing season in the field. Three experimental fields were considered and the applied experimental design was a strip plot with three replicates; rice samples were collected at four different growing stages. The efficacy of the fungicide treatment on rice fungal population was demonstrated with around 20% less total fungal incidence in sprayed samples compared to untreated ones; the same decrease was noted also in Fusarium spp. species but not in Aspergillus versicolor. Of the mycotoxins considered, ochratoxin A (OTA) and aflatoxins (AFBs) were never detected, deoxynivalenol (DON) was found in 46% of samples at levels always lower than 100 µg/kg, while sterigmatocystin (STC) occurred in all the paddy rice samples collected after flowering, with a maximum value of 15.5 µg/kg. Treatment with azoxystrobin was not effective in reducing DON contamination, but it had an important and significant effect on STC content, showing a decrease of 67% in the sprayed samples.

Mitigation measures for acrylamide reduction in dough-based potato snacks during their expansion by frying.

Acrylamide (AA) can occur in fried and baked food products which contain reducing sugars and free asparagine. Recently, the European Commission established mitigation measures and benchmark levels for the reduction of AA in food. The content of reducing sugars in raw materials and the temperature and time of the expansion process by frying were considered in this study of the preparation of dough-based potato snacks, mainly destined for children. Final moisture and bulk density were also evaluated. An increase from 0.15 to 1.0% in reducing sugar content, due to the addition of micro-ingredients in the dough, caused a remarkable AA increase of five- to six-fold. During frying at temperatures between 175 and 195°C, AA was produced after only a few seconds; the AA content was affected more by process time than by temperature. The best temperature/time conditions for expansion by frying were 185°C for 8 s.

Survey on acrylamide in roasted coffee and barley and in potato crisps sold in Italy by a LC-MS/MS method.

A survey on the occurrence of acrylamide (AA) in roasted coffee, barley, and potato crisps was carried out using an intra-lab validated liquid chromatography (LC)-MS (mass spectrometry)/MS method. Over the years 2015-2016, 66 samples of coffee, 22 of roasted barley, and 22 of potato crisps were collected from retail outlets in Italy. AA was detected in almost all samples. In roasted coffee, the level exceeded 450 µg kg-1, the limit recommended by the European Commission (EC), in 36.4% of the samples. In roasted barley, mean contamination was slightly lower than in coffee and no sample exceeded the EC limit of 2000 µg kg-1. The AA contamination in potato crisps was remarkable. A percentage of 36.4 (n = 8) showed a value higher than the EC limit of 1000 µg kg-1. Considering the average consumption of coffee and potato crisps by Italian people, AA exposure is significant and should be decreased.

Sterigmatocystin Occurrence in Paddy and Processed Rice Produced in Italy in the Years 2014-2015 and Distribution in Milled Rice Fractions.

The occurrence of sterigmatocystin (STC) in paddy and processed rice samples produced in Italy was surveyed. After extraction and purification, STC was analysed using HPLC-MS/MS. STC was detected in all paddy rice samples (n = 49), in the range 0.29-15.85 µg·kg-1. As regards processed rice, a widespread contamination was found in brown and parboiled rice. All the brown rice samples were contaminated between 0.12 and 1.32 µg·kg-1; for parboiled rice, the incidence was 90.9% and the maximum level was 1.09 µg·kg-1. The contamination in white rice was significantly lower (p < 0.01). The STC distribution in different rice fractions, obtained by the de-hulling and polishing processes, was evaluated. After de-hulling, the STC percentage remaining in brown rice was in the range 21.2%-30.8%. The polishing process, from brown to white rice, caused another remarkable decrease of contamination; the STC remaining in white rice was 2.2%-8.3% of the amount found in paddy rice.

Enzyme-assisted extraction for the HPLC determination of aflatoxin M1 in cheese.

The extraction of aflatoxin M1 (AFM1) from cheese is generally carried out using chlorinated organic solvents. In this study, two innovative methods were developed, based on an enzyme-assisted (EA) extraction using proteolytic enzymes (pepsin or pepsin-pancreatin). After purification through an immunoaffinity column, AFM1 is determined by HPLC-FLD. A comparison between the new EA methods and an established chloroform (CH) method was carried out on 24 cheese samples. The results showed that the extraction efficiency of the EA methods was independent of ripening time of cheese, whereas the CH method was not able to fully recover AFM1 from ripened cheeses. The simpler (pepsin) of the two methods has been adopted by our laboratory for routine analysis of AFM1 in cheese. In comparison with the CH method, the pepsin-HCl (P-HCl) method is simpler, avoiding solvent evaporation, dissolution and partition in a separating funnel; moreover, it gives higher recoveries, comparable LOD and LOQ and more accurate results.

Plasma ochratoxin A levels, food consumption, and risk biomarkers of a representative sample of men and women from the Molise region in Italy.

BACKGROUND: Ochratoxin A (OTA) is a mycotoxin present in food that can be found in human blood, due to its long half-life. Plasma OTA detection represents a good parameter for evaluating the exposure at the population level. PURPOSE: The relation between plasma OTA levels, dietary habits, and specific disease risk biomarkers (body mass index (BMI), C-reactive protein (CRP), and cardiovascular risk score) was investigated. METHODS: The study involved 327 subjects (150 men and 177 women) aged between 38 and 48 years. Food consumption was evaluated by means of the EPIC questionnaire; plasma OTA was measured by HPLC; CRP was determined in fresh serum samples by a latex particle-enhanced immunoturbidimetric assay. RESULTS: OTA was detected in 99.1% of plasma samples (LOD 25 ng/L); the mean ± SD value was 0.229 ± 0.238 ng/mL. However, only 5.2% of samples exceeded 500 ng/L, considered the threshold for a possible pathogenic activity. The estimated mean daily dietary intake of OTA resulted 0.452 ± 0.468 ng/kg body weight (bw)/day, markedly lower than the tolerable daily intake set by EFSA (17.1 ng/kg bw/day). Processed and mutton/lamb meat were found to contribute most to plasma OTA variance. Nevertheless, cereals, wine, beer, and jam/honey consumption correlated positively with OTA levels. Plasma OTA showed a significant positive association with CRP and cardiovascular risk score (ß = 0.20 ± 0.08; P = 0.015 and ß = 0.25 ± 0.08; P = 0.001, respectively); however, the association was present in men but not in women. CONCLUSIONS: Even if the hypothesis of a possible hepatic toxicity of OTA in humans is yet to be verified, the positive association between plasma OTA and CRP may indicate a possible role of OTA in inflammation status and consequently in the genesis of cardiovascular diseases and cancer.