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Starches-rich and protein-rich cereal samples commonly need tedious sample preparation steps before instrumental analysis. This study developed a miniaturized centrifugal integrated cold-induced phase separation (CIPS) method for convenient sample preparation. A small-sized centrifuge tube (2 mL) and a low-temperature centrifuge, both of which are easily accessible, make up the basic components of the system. Unlike conventional sample preparation methods that need a step-by-step extraction, enrichment, purification, and centrifugation, this centrifugal integrated CIPS method can be performed by a one-step combination protocol under a low-temperature centrifuge. As a proof-of-concept study, satisfactory recoveries and enrichment factors were demonstrated for the extraction of fumonisins and ochratoxins from cereals. A sensitive and selective quantification method was yielded by combining LC-HRMS using tSIM acquisition mode, with good linearity (R 2  > 0.998), accuracy (82.9-106.5%), and precision (<13.4%). This strategy is convenient, low-cost, repeatable, and easy to semi-automate, further expanding the extraction potential for other acidic mycotoxins., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Ltd. All rights reserved.)

Fusarium verticillioides, a major fungal pathogen of maize, produces fumonisins, mycotoxins of global food safety concern. Control practices are needed to reduce the negative health and economic impacts of fumonisins. Therefore, we investigated volatile organic compounds (VOCs) emitted by fumonisin-producing (wild-type) and nonproducing (mutant) strains of F. verticillioides. VOC emissions were analyzed by gas chromatography-mass spectrometry following inoculation of maize kernels, and fumonisin accumulation was analyzed by high-performance liquid chromatography. Mutants emitted VOCs, including ethyl 3-methylbutanoate, that the wild type did not emit. In particular, ANOVA analysis showed significant differences between mutants and wild type for 4 VOCs which emission was correlated with absence of fumonisins. Exogenous ethyl 3-methylbutanoate reduced growth and fumonisin production in wild-type F. verticillioides, showing its potential in biocontrol. Together, our findings offer valuable insights into how mycotoxin production can impact VOC emissions from F. verticillioides and reveal a potential biocontrol strategy to reduce fumonisin contamination., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Ag 3 PO 4 nanoparticles (NPs) was prepared through a facile coprecipitation method, and was first found to have excellent laccase-mimicking catalytic activity. The study confirms that Fumonisin B1 (FB1) can effectively hinder the production of superoxide anion (O 2 - ) between Ag 3 PO 4 NPs and dissolved oxygen, and further inhibit laccase-mimicking activity of Ag 3 PO 4 NPs. Thus, a novel rapid colorimetric sensor for FB1 analysis in cereal was first established using laccase-mimicking activity as sensing signal. The absorbance variation of sensing solution is directly related to the amount of FB1, and the color change is further combined with smartphone for quantitively analysis of FB1. The limit of detection (LOD) of the sensor is determined as low as 1.73 μg·L -1 , which is far lower than the maximum residue limits (MRLs) of FB1 set by European Commission and US Food and Drug Administration (FDA). The average recovery of 87.8-104.5% for FB1 detection was obtained in cereal., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

In this study, based on the high-throughput automatic sample pretreatment with immunoaffinity magnetic beads with oriented immobilized antibodies, grain and feed fumonisin (FB) content was detected using pre-column automatic derivatization of high-performance liquid chromatography (HPLC). The FB capacity of well-oriented antibody immunoaffinity magnetic beads was 1.5-1.8 times that of magnetic beads with randomly fixed antibody. This pre-column automatic derivatization method using an autosampler can reduce error from manual injection and improve detection efficiency. The spiked recoveries for three different concentrations in maize, husked rice, and pig feed under optimized conditions were 84.6-104.0% (RSD < 9.3%). Our novel method was also applied to the analysis of FBs in 63 maize samples collected from the main maize-production regions in China. The results showed that as latitude increased, the contamination level of FBs tended to decrease. High temperature and high humidity are also more favorable for FB growth., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier Ltd. All rights reserved.)

Fumonisin B 1 (FB 1 ), the most occurring fumonisin, is capable of disrupting sphingolipid metabolism and poses a serious threat to human and animal health. The high incidence and toxicity of FB 1 have created an urgent need for alternative quantitative determination strategies. Herein, a colorimetric aptasensor was developed by combining the catalytical metal-organic frameworks with the polyacrylamide-DNA hydrogel. The porphyrin-based MOF provided the aptasensor with robust peroxidase-like activity while maintaining good stability. Concurrently, the polyacrylamide-DNA hydrogel constructed via strand-induced hybridization chain reaction (HCR) endowed the aptasensor with outstanding stimuli-responsiveness towards FB 1 molecules. The developed aptasensor demonstrated remarkable selectivity and ease of use for assays conducted in solution and food samples. It also exhibited superior analytical performance with a linear range of 0.05-100 ng mL -1 and a limit of detection (LOD) of 0.024 ng mL -1 . The strategy could serve as a model to develop diverse stimuli-responsive aptasensors targeting hazards in food safety., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022. Published by Elsevier Ltd.)

A "turn-on" fluorescence sensor was developed for total detection of fumonisin B 1 , B 2 and B 3 (FB 1 , FB 2 and FB 3 ) in maize samples. Rhodamine B isothiocyanate (RBITC) and gold nanoparticles (AuNPs) were employed as the energy donor-acceptor pairs. The intensity of restored fluorescence was inversely proportional to the concentration of the FBs. The limit of detection (LOD) of the sensor for FB 1 was 23.80 pg/mL. The coefficient of variation (CV) was both less than 7% for intra- and inter-assay. The linear range was from 51.39 to 2125.92 pg/mL. The average recoveries of FBs from maize samples were ranged from 88.7% to 107.2%. The correlation coefficient of the results between the developed sensor and LC-MS/MS was 0.9970. To fulfill the procedure of the assay, only 46 min was needed. These results suggest that the fluorescence "turn-on" sensor has great potential applications in the analysis of FBs in maize samples., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

A rapid and sensitive immunochromatographic strip (ICS) based on a single-chain variable fragment (scFv) was developed for detecting fumonisin B 1 (FB 1 ). The ICS was based on a competitive reaction for colloidal gold-labeled scFv between FB 1 and FB 1 -BSA, which was used along with sheep anti-mouse IgG as capture reagents immobilized at test and control lines, respectively, on a nitrocellulose membrane of the strip. The limit of detection of the ICS was 2.5 ng/mL (25 μg/kg) FB 1 in buffer, and the sensitivity was eight times higher than that of monoclonal antibodies for the preparation of the scFv. The cross-reactivity of the scFv with common mycotoxins was determined by ICS, the results showed that the scFv were not against other mycotoxins. Eight naturally contaminated maize samples were analyzed with the scFv-based ICS and by LC-MS/MS. The results of analysis obtained with the strip assay showed good agreement with those obtained by LC-MS/MS., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Beer is one the most consumed alcoholic beverage in the world and its contamination with mycotoxins is of public health concern. This study reports a fast and automated analytical procedure based on a multi-heart-cutting two-dimensional liquid chromatography tandem mass spectrometry method using electrospray ionization for the determination of seven mycotoxins (aflatoxins B1, B2, G2 and G1, ochratoxin A, fumonisins B1 and B2) in beers. The developed method was based on the heart-cutting 2D- HPLC technique in which only the specific portions of the first dimension, in the retention time of analytes, were transferred into the second dimension for the further separation and successive determination. The method uses two different chromatographic columns; in the first dimension, 50 μL of sample was injected on first column, and mycotoxins elution regions were collected in a loop and transferred into the second column for the separation of analytes. Each column operated in gradient elution mode in order to eliminate interfering compounds and improve separation and peak shape. After the optimization, the method has been validated according to EU regulation and finally applied for the analysis of forty beer samples collected from Italian supermarkets. Among all mycotoxins studied, fumonisins B1 was the most widely distributed in analysed beers (>21%) in the range from 0.6 to 12.3 ng mL -1 . The automated methodology developed was able to determine accurately and simultaneously seven mycotoxins in beer. This provided a significant reduction of sample handle and, consequently of analysis time., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

Fumonisins (FBs) exist widely in crops, foods and feeds. Consumption of FBs contaminated corn can cause oesophageal cancer. So it is necessary to develop sensitivity methods for its detection. Here, we report an enhanced assay for rapid and ultra-sensitive detection of FBs based on nanomagnetic beads (NMBs) and antibody-biotin-streptavidin-HRP. Because antibody-BNHS can bind with several number of streptavidin-HRP, the signal amplification of the catalytical oxidation of TMB was enhanced. The detection limit of sensor was down to 0.21 ng mL -1 with a linear range from 0.31 to 162.42 ng mL -1 . Since NMBs provide a nearly "in solution" reaction, they lead to a shortened reaction time (22 min) than that of flat solid-phase based traditional assay. Furthermore, the recoveries obtained by standard FBs spiked to maize samples were from 100.6 to 107.3%. This enhanced assay supplied a rapid, sensitive and reliable method for detection of FBs in maize., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020. Published by Elsevier Ltd.)

The need for safe and quality food, free from the presence of hazardous contaminants such as mycotoxins is an on-going and complex challenge. Cold atmospheric pressure plasma (CAPP) has the potential to contribute to achieving this goal. Decontamination efficacy of CAPP against six of the most common mycotoxins found in foods and feedstuffs was assessed herein. Concentration reduction of up to 66% was achieved in maize for both aflatoxin B 1 and fumonisin B 1 . Degradation products were detected only in the case of aflatoxin B 1 and zearalenone and were tested on human hepatocarcinoma cells with no increase in cytotoxicity observed. Analysis of treated maize revealed substantial changes to small molecular mass components of the matrix. While CAPP shows promise in terms of mycotoxin detoxification important questions concerning potential changes to the nutritional and safety status of the food matrix require further investigations., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Fumonisin B1 (FB1) is a carcinogenic mycotoxin produced by Fusarium species contaminating maize. At present, fumonisin determination is performed using costly and demanding chromatography techniques or immunoassays. Recently, a molecularly imprinted polymer nanoparticles (nanoMIPs) - based assay (MINA) has been developed for FB1 detection. Herein, we have applied MINA for the determination of FB1 in naturally contaminated maize samples and results were compared with those obtained with ELISA and a reference HPLC method (AOAC No. 2001.04). The nanoMIPs as a recognition element mimicking antibodies used in ELISA were produced by solid phase synthesis and used in MINA for FB1 determination in 53 maize samples. As a result, 18 maize samples were contaminated with FB1 at levels higher than 0.25 mg/kg. Fumonisin concentrations from samples measured by MINA were well correlated with those using ELISA and HPLC. Therefore, MINA could be used as an alternative technique for FB1 determination in maize., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

In this report, a UPLC-ESI-MS/MS method for the simultaneous determination of aflatoxins, ochratoxin A, zearalenone, deoxynivalenol, fumonisins, T-2 and HT-2 toxins, fusarenone X, diacetoxyscirpenol, and 3- and 15-acetyldeoxynivalenol in feedstuffs was developed. A quadrupole-time-of-flight mass spectrometer detector (QTOF-MS) operating in full scan mode was combined with the UPLC-ESI-MS/MS system to confirm the identity of detected mycotoxins and to identify other possible microbial metabolites occurring in samples. Sixty-two feed samples from the Spanish market were analyzed. Extraction of metabolites was carried out with acetonitrile-water-formic acid (80:19:1, v/v/v). Method detection and quantification limits and performance criteria set by Commission Regulation (EC) No 401/2006 were fulfilled. Relatively high levels of the main regulated mycotoxins and presence of non-regulated mycotoxins in feed samples were found. This is the first study in which mycotoxins and other microbial metabolites occurring in feed are studied using a UPLC-QTOF-MS system being therefore a reference report., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Pre-column derivatization with 9-fluorenylmethyl chloroformate (FMOC-Cl) was determined to be effective for quantitation of fumonisins B 1 and B 2 in feed. Liquid-solid extraction, clean-up using immunoaffinity solid phase extraction chromatography, and FMOC-derivatization preceded analysis by reverse phase HPLC with fluorescence. Instrument response was unchanged in the presence of matrix, indicating no need to use matrix-matched calibrants. Furthermore, high method recoveries indicated calibrants do not need to undergo clean-up to account for analyte loss. Established method features include linear instrument response from 0.04-2.5µg/mL and stable derivatized calibrants over 7days. Fortified cornmeal method recoveries from 0.1-30.0μg/g were determined for FB 1 (75.1%-109%) and FB 2 (96.0%-115.2%). Inter-assay precision ranged from 1.0%-16.7%. Method accuracy was further confirmed using certified reference material. Inter-laboratory comparison with naturally-contaminated field corn demonstrated equivalent results with conventional derivatization. These results indicate FMOC derivatization is a suitable alternative for fumonisins B 1 and B 2 quantitation in corn-based feeds., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

The aim of this study was to evaluate the fate of fumonisins B 1 (FB 1 ) and B 2 (FB 2 ) during industrial dry-milling in two lots from 2014 (n=120) and 2015 (n=120) of non-transgenic corn and their fractions (germ, pericarp, endosperm, cornmeal and grits), collected from one of the major Brazilian milling industries. Fumonisins were concentrated in the germ and pericarp at a rate of 322% and 188% (lot 1) and 311% and 263% (lot 2), respectively. In the endosperm, cornmeal and grits fumonisin levels decreased from 60 to 95%. Fumonisin levels in cornmeal and grits were below the maximum limit tolerated by the European Commission. Therefore, corn industrial dry-milling can contribute to reducing fumonisin levels in corn products intended for human consumption., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The simultaneous quantification of 15 mycotoxins in cow milk by liquid chromatography-mass spectrometry, is presented. Extraction was performed with acidified acetonitrile, followed by a cleanup step with sodium acetate. During validation limits of detection (LOD) and quantification, linearity, precision, accuracy, recovery, matrix effect, and stability were studied. LOD values were between 0.02 and 10.14ng/mL for aflatoxins M1, B1, B2, G1, G2, ochratoxins A and B, HT-2 and T-2 toxins, deepoxy-deoxynivalenol, zearalenone, sterigmatocystin and fumonisins B1, B2 and B3. Recovery values were between 82.6 and 94.4% for all the mycotoxins, except for fumonisins. The recovery values for fumonisins were between 42.1% and 64.6%. Matrix effect, between 25.5 and 96.8%, appeared for all of the mycotoxins, especially for deepoxy-deoxynivalenol, zearalenone and sterigmatocystin. The validated method achieves the quantification of those mycotoxins of major concern and mycotoxins that are not frequently studied in milk, such as fumonisins, sterigmatocystin or ochratoxin B., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Worldwide, barley is the main source of carbohydrate in the brewing process. However, corn is often used as an adjunct to improve and accelerate the fermentation process. Considering that, these two substrates are susceptible to fungal contamination as well as mycotoxins. The objective of the current study is to determine the incidence of the mycotoxins deoxynivalenol (DON) and fumonisin B 1 (FB 1 ) in industrial beers. The method applied for mycotoxin analyses included high performance liquid chromatography . The mean levels for recovery experiments were 89.6% for DON and 93.3% for FB 1 . DON was not detected in any of the analyzed samples whereas FB 1 was found in 49% of the 114 samples. The current survey demonstrated levels of FB 1 contamination in industrial beer, possibly due to the addition of contaminated adjuncts. It is necessary to establish maximum levels of mycotoxins in beer in Brazil and other countries in order to reduce health risks., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The effect of nixtamalization on the content of fumonisins (FBs), hydrolysed (HFBs) and partially hydrolysed (PHFBs) fumonisins in maize was investigated at laboratory-scale. Maize naturally contaminated with FBs and PHFBs was cooked with lime. Starting raw maize, steeping and washing waters and final masa fractions were analysed for toxin content. Control-cooking experiments without lime were also carried out. The nixtamalization reduced the amount of FBs and PHFBs in masa and converted them to HFBs. However, the three forms of fumonisins collected in all fractions amounted to 183%, indicating that nixtamalization made available forms of matrix-associated fumonisins that were then converted to their hydrolysed forms. Control-cooking enhanced FBs and PHFBs reduction, due to the solubility of fumonisins in water during the steeping process, but did not form HFBs. These findings indicate that benefits associated with enhancing the nutritional value of nixtamalized maize are also associated with a safer product in terms of fumonisin contamination., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

Corn plants contaminated with Fusarium verticilloides were harvested at two dates and ensiled in laboratory silos. The stability of Fumonisins B1 and B2 (FB1, FB2) was studied and the effects of inoculant use (Lactobacillus buchneri) and of the ensiling time were assessed. The occurrence of masked fumonisins was also investigated. After the extraction of the free forms (FB1, FB2), the residue was subjected to an alkaline hydrolysis resulting in the release of derivates subsequently detected by LC-HESI-MS/MS. The ensiling time has shown to be a significant factor for the evolution of free FB1 and FB2 at the 2nd harvest date. Moreover, the use of inoculant had a significant effect on the stability of hidden and total FB1 at the two harvest dates. Samples previously ensiled and exposed to aerobic conditions for 7days have shown higher fumonisin levels than those not exposed to air. Our results showed that 65% and 39% of the total FB1 and FB2 contents in silage were due to hidden fumonisins., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

The industrial use of barley grain has experienced continuous growth, mainly due to its economic importance for malt production. From a technological perspective, fungal persistence can reduce product marketability and cause economic losses. In this sense, the aim of the present study was to determine the presence and identification of mycoflora and the occurrence of deoxynivalenol (DON) and fumonisins (FBs) in malting barley. The samples presented a low count of fungal colonies, with values ranging from 10.5 to 0.5 × 10(1)CFU g(-1) and the species most found were Fusarium graminearum and Fusarium verticillioides with 26% and 12% of incidence, respectively. In the samples analyzed for mycotoxins occurrence, DON and FBs were present in 18% and 12%, respectively. The high concentrations of toxins found in the malting samples may be strongly influenced by agricultural practices and the weather conditions during critical phases of plant growth., (Copyright © 2015 Elsevier Ltd. All rights reserved.)

The chemical composition of Rosmarinus officinalis L. essential oil (REO) was analysed by gas chromatography-mass spectrometry and nuclear magnetic resonance spectroscopy. The main compounds of the REO were 1.8 cineole (52.2%), camphor (15.2%) and α-pinene (12.4%). The mycelial growth of Fusarium verticillioides (Sacc.) Nirenberg was reduced significantly by 150 μg/mL of REO. Significant microscopic morphological changes were visualised, such as the rupture of the cell wall and the leakage of cytoplasm at 300 μg/mL of REO. At lower concentrations of REO, the effects on the production of ergosterol and the biomass of mycelium varied, as did the effects on the production of fumonisins, but at ≥300 μg/mL of REO, these processes were significantly inhibited, showing the effectiveness of the REO as an antifungal agent. The results suggested that the REO acts against F. verticillioides by disrupting the cell wall and causing the loss of cellular components, subsequently inhibiting the production of fumonisins and ergosterol., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

In this study, fumonisin B1 (FB1) consumption was assessed through determination of FB1 in corn meal, corn flour, corn flakes, polenta, canned corn and popcorn collected from homes of residents of Pirassununga, São Paulo, Brazil, and using a Food Frequency Questionnaire (FFQ) filled out by the residents. One hundred and twenty samples were collected from 39 residents on four separate occasions. FB1 was determined by high performance liquid chromatography using a validated method that uses SAX column clean-up. The highest levels of FB1 were found in corn meal at a mean concentration of 474.6 μg kg(-1). However, none of the samples tested for FB1 had levels above the tolerance limit established in Brazil. The mean probable daily intake (PDIM) of FB1 was 63.3 ng kg(-1)body weight day(-1), which is approximately 3% of the provisional maximum tolerable daily intake (PMTDI) recommended for fumonisins., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

Fumonisins are mycotoxins produced by Fusarium species that commonly live in maize. Whereas fungi damage plants, fumonisins cause disease both to cattle breedings and human beings. Law limits set fumonisins tolerable daily intake with respect to several maize based feed and food. Chemical techniques assure the most reliable and accurate measurements, but they are expensive and time consuming. A method based on Near Infrared spectroscopy and multivariate statistical regression is described as a simpler, cheaper and faster alternative. We apply Partial Least Squares with full cross validation. Two models are described, having high correlation of calibration (0.995, 0.998) and of validation (0.908, 0.909), respectively. Description of observed phenomenon is accurate and overfitting is avoided. Screening of contaminated maize with respect to European legal limit of 4 mg kg(-1) should be assured., (Copyright © 2013 Elsevier Ltd. All rights reserved.)

Fourier transform near infrared (FT-NIR) spectroscopy is an analytical procedure generally used to detect organic compounds in food. In this work the ability to predict fumonisin B(1)+B(2) contents in corn meal using an FT-NIR spectrophotometer, equipped with an integration sphere, was assessed. A total of 143 corn meal samples were collected in Friuli Venezia Giulia Region (Italy) and used to define a 15 principal components regression model, applying partial least square regression algorithm with full cross validation as internal validation. External validation was performed to 25 unknown samples. Coefficients of correlation, root mean square error and standard error of calibration were 0.964, 0.630 and 0.632, respectively and the external validation confirmed a fair potential of the model in predicting FB(1)+FB(2) concentration. Results suggest that FT-NIR analysis is a suitable method to detect FB(1)+FB(2) in corn meal and to discriminate safe meals from those contaminated., (Copyright © 2012 Elsevier Ltd. All rights reserved.)