Deoxynivalenol In Wheat Flour Research Articles

Surface-enhanced Raman detection of deoxynivalenol allenol in agricultural products

Fungal toxins are secondary metabolites of fungi. Food is highly susceptible to contamination by various fungal species that produce fungal toxins during production and storage. Fungal toxins can cause either acute or chronic poisoning from long-term, low-dose ingestion. Therefore, fungal toxins have become a topic of international interest as a food safety issue. Deoxynivalenol (DON) is a single-terminal sporam toxin produced predominantly by Fusarium graminae and Fusarium pinkosa. DON is globally one of the most common fungal toxins contaminating grain, food, and feed. Various methods have been applied for screening and detecting DON; however, these methods utilize expensive instruments and entail complex operations, poor repeatability, and low sensitivity. Therefore, the development of a simpler, more rapid, and sensitive sensing technology for DON detection is important for applications within the agriculture and food industry. Recently, surface-enhanced Raman scattering (SERS) has become a rapidly developing spectral analysis technology with unique advantages, including high sensitivity, high throughput, and rapid response rates. Therefore, attempts have been made to apply the SERS technique to detecting DON. However, due to the limitations concerning SERS substrates, the currently established SERS method exhibits serious problems, including low sensitivity and weak anti-interference ability, and cannot meet the requirements of sample detection. Recently, our group has prepared aggregated silver nanoparticles (a-AgNPs/CDs) with high SERS activity by using single-layer carbon-based dots (CDs) as a capping agent. Moreover, the obtained materials (a-AgNPs/CDs) were combined with hydrogel technology to prepare novel hydrogel SERS chips. The obtained SERS chips exhibited several advantages over traditional SERS substrates, such as high sensitivity, long-term stability, improved uniformity, and strong anti-interference capabilities. Herein, a novel SERS method for rapid screening and detection of DON in grains was established using a portable Raman spectrometer based on the developed hydrogel SERS chips. The main experimental conditions were optimized before the SERS detection of DON; this included the optimization of the hydrogel SERS chip soaking temperature and time in the DON solution. It was found that the optimal soaking temperature and time were 40 ℃ and 5 min, respectively. Under the optimal SERS detection conditions, the linear response range of DON was 1-10000 μg/kg (correlation coefficient (R2)=0.9967), and the limit of detection (LOD) was 0.14 μg/kg. Due to the unique pore size structure of the hydrogel, common sugar, protein, oil, pigment, and other interfering substances in the sample matrix were blocked outside the hydrogel. Therefore, only simple extraction was required while detecting complex samples. This method was applied to detecting DON in wheat flour, yielding recoveries of 97.3%-103% with relative standard deviations of 4.2%-5.0%. The established SERS method for DON detection exhibits a broader response range, high sensitivity, good repeatability, rapid response, simple operation, and strong anti-interference capability. This shows that the laboratory-constructed hydrogel SERS chip has excellent potential for rapid screening and detection of biotoxins in food.

Survey of the Presence of Nivalenol and Deoxynivalenol in Wheat Flour Factories of Khuzestan Province, Iran

Background: Wheat is frequently contaminated by Deoxynivalenol (DON) and Nivalenol (NIV), which are type B trichothecenes produced by Fusarium fungi. Most problems related to these contaminants involve prolonged feed intake at low levels of contamination. This study investigated the occurrence of NIV and Deoxynivalenol (DON) in wheat flour in flour factories in Khuzestan Providence, Iran. Methods: In total, 104 samples were collected in this study. An acetonitrile/water mixture (84:16, v/v) was used to extract the samples. The extracts were filtered and purified using a Whatman No. 4 paper and MycoSepTM 227 column. Then, they were evaporated to dryness at 40˚C under a nitrogen stream. After dissolving the dry residue in the mobile phase, containing a mixture of methanol, acetonitrile, and water (5:5:90, v/v/v), the contents of NIV and DON in the samples were measured in High-Performance Liquid Chromatography (HPLC) system with a column C18 (150 mm×4.6 mm ID, 5 μm) and a UV detector (220 nm). Results: The results showed that among 104 wheat flour samples, 28 (26.8%) and 54 (51.9%) samples were contaminated with NIV and DON, respectively. The mean and maximum concentrations were 118.75 and 2278 ng/g for NIV, and 593 and 67.88 ng/g for DON, respectively. Conclusion: Based on the findings, DON and NIV had significantly lower concentrations than the maximum tolerated level (1 μg/g), established by the Institute of Standards and Industrial Research of Iran. Therefore, there were no health risks for consumers at the studied contamination levels.

Adulteration identification of wheat flour in chestnut flour based on differences in mycotoxin contamination by liquid chromatography-tandem mass spectrometry

建立了分散固相萃取-超快速液相色谱-串联质谱法同时测定板栗粉和小麦粉中43种真菌毒素的方法,对48份板栗粉和80份小麦粉样品的污染状况进行调查,筛选出5种专属于小麦粉的标志性真菌毒素。样品采用84%(v/v)乙腈水溶液提取,提取液采用C18结合增强型脂质去除净化剂(EMR-Lipid)净化,采用响应曲面-中心组合设计优化分散固相萃取净化方法。净化液在BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)上分别采用0.1%甲酸水溶液和含0.1%甲酸的甲醇-乙腈(1:1, v/v)(电喷雾正离子模式)、水和乙腈(电喷雾负离子模式)为流动相进行梯度洗脱,分别采用电喷雾电离(ESI)正负离子模式检测,基质匹配曲线外标法定量。板栗粉中真菌毒素的3水平加标回收率在72.4%~109.4%之间,相对标准偏差(RSD)<7.5%;小麦粉中真菌毒素的3水平加标回收率在70.7%~112.9%之间,RSD<9.3%;两种基质中43种真菌毒素的定量限均在0.1~20.0 μg/kg之间,方法线性相关系数均大于0.9991。利用所建立的方法监测了128份样品,结果表明,两种基质普遍受到真菌毒素污染,其中脱氧雪腐镰刀菌烯醇及其衍生物3-乙酰化-脱氧雪腐镰刀菌烯醇、15-乙酰化-脱氧雪腐镰刀菌烯醇、雪腐镰刀菌烯醇、去环氧-脱氧雪腐镰刀菌烯醇仅在小麦粉中检出。采用GB 5009.111-2016同位素稀释液相色谱-串联质谱法验证,检测结果与本方法一致。所建立的方法简便、快速、灵敏、准确,可有效满足板栗粉和小麦粉中真菌毒素残留的检测要求,脱氧雪腐镰刀菌烯醇及其4种衍生物可以作为两种食品的掺假标志物。

Near-infrared spectroscopy as a tool for rapid screening of deoxynivalenol in wheat flour and its applicability in the industry

ABSTRACT This study aimed to evaluate the applicability and efficiency of Near-Infrared Spectroscopy (NIR) by using dispersive NIR and Fourier Transform NIR to analyse 267 samples of Brazilian wheat flour contaminated with deoxynivalenol (DON). For this, Partial Least-squares Discriminant Analysis (PLS-DA) and Principal Component Analysis-Linear Discriminant Analysis (PC-LDA) were used as discriminatory methods. Next, the samples were classified according to the maximum tolerated limits (MTL) for DON in Brazil, 750 μg kg−1, and two groups were established for the calibration set: category A (≤450 μg kg−1), non-contaminated or below the MTL; and category B (>450 μg kg−1), contaminated or above the MTL. Validation samples through PLS-DA showed correct classification rates in the range of 85–87.5% and presented a 10–15% error; for PC-LDA, the hit rate was over 85% with an error of 10–15%. The present findings demonstrate that NIR is an excellent alternative method to classify wheat flour samples according to DON content.

Direct qualitative and quantitative determination methodology for massive screening of DON in wheat flour based on multi-molecular infrared spectroscopy (MM-IR) with 2T-2DCOS

Deoxynivalenol (DON) contamination in wheat flour induces a number of adverse health effects to consumers and livestock, even at very low concentrations. Direct detection methods for massive screening of DON in wheat flour is still lacking. A new methodology integrating multi-molecular infrared spectroscopy (MM-IR) with two-trace two-dimensional correlation spectroscopy (2T-2DCOS) was developed for in-situ qualitative and quantitative determination of DON in wheat flour as a whole. Typical spectral variation of wheat flour samples with diverse concentration of DON were stepwise characterized by MM-IR and tiny spectral profile differences resulting from concentration variation of DON were visually disclosed by 2T-2DCOS. Based on the obtained key spectral features of DON, 180 of wheat flour samples with DON higher and lower than 1.00 mg/kg were undoubtedly classified by Principal Component Analysis (PCA) and Support Vector Machines (SVM) with an accuracy rate up to 100% (for Second derivative spectra consisted of selected bands, SD-SS). Furthermore, a robust quantitative prediction model was established based on partial least squares (PLS) of SD-SS (Rc: 0.998, RMSEC: 0.135; Rp: 0.968, RMSEP: 0.421), and its excellent predictive capacity of model was validated by both residual prediction deviation (RPD) value of 3.2 and t-test. It was demonstrated that the developed methodology was applicable for screening and quantitative detection of DON in wheat flour based on the novel correlation analysis methods (SD-2DCOS-IR and 2T-2DCOS-IR) with chemometrics tools, which could be utilized both at laboratory and industrial level for quality control purposes of a large wheat flour sample set.

Action of Bacillus natto 16 on deoxynivalenol (DON) from wheat flour.

The aim of this research is to study the removal characteristics and evaluate the detoxify action of deoxynivalenol by Bacillus natto 16 in wheat flour as food or feed. The content of deoxynivalenol was determined using ELISA by testing the deoxynivalenol removal rate, and the influence of culture supernatant, intracellular substances, crude enzyme and cell wall on the deoxynivalenol in wheat flour was studied. The effect of bacterial components on the removal of deoxynivalenol was studied in the artificial gastrointestinal environment to simulate the digestion of food. Secondary metabolites were analysed by high-performance liquid chromatography in tandem with mass spectrometry (HPLC-MS). The cell wall can reduce the content of deoxynivalenol in the sample by adsorption, the influence of culture supernatant, intracellular substances and crude enzyme can convert deoxynivalenol into substances with a lower molecular weight. Bacterial components have no effect on deoxynivalenol in wheat flour in simulated gastric fluid (SGF) and have a certain removal effect on deoxynivalenol, which is closely related to intestinal digestion time and pH, in simulated intestinal fluid. Experimental results indicate that the removal of deoxynivalenol by B. natto 16 includes adsorption and biodegradation, SGF would invalidate the deoxynivalenol removal activity of B. natto 16's components. Our study showed that as an edible probiotic bacterium, B. natto 16 can effectively remove deoxynivalenol from wheat flour as food or feed, and can be used as a new deoxynivalenol -detoxifying microbe. The results of this research could provide the theory foundation for further development and application of B. natto 16.

Incidence of Deoxynivalenol in Wheat Flour in Argentina and GC–ECD Method Validation

Abstract Background: Deoxynivalenol (DON) is a mycotoxin produced mainly by Fusarium graminearum. This fungus is the main plant pathogen associated with Fusarium Head Blight (FHB) wheat disease, causing significant economic losses and exposing human population to severe health risks. DON production changes widely among different years and areas and its effects are larger in years with abundant rainfall and high relative humidity. To date, Argentina has not established DON tolerance limits. Objective: To validate a method using GC with electron capture detector (GC-ECD) and to provide evidence of DON contamination in Argentinean commercial wheat flour. Results: A total of 34 different flour samples were analyzed obtaining 91.2% of incidence with a mean level of 243 µg/kg and a median level of 165 µg/kg. The method showed acceptable LOD (24 µg/kg) and LOQ (79 µg/kg), relative SD (RSD) of the intermediate precision (RSD = 5.98%), recovery (89.3%) and uncertainty (14%). Conclusions: The method was successfully validated according to the studied parameters. Incidence results for DON contamination are low and in accordance with previous studies for years with low FHB incidence in wheat.

Incidence of Deoxynivalenol in Wheat Flour in Argentina and GC-ECD Method Validation.

Background: Deoxynivalenol (DON) is a mycotoxin produced mainly by Fusarium graminearum. This fungus is the main plant pathogen associated with Fusarium Head Blight (FHB) wheat disease, causing significant economic losses and exposing human population to severe health risks. DON production changes widely among different years and areas and its effects are larger in years with abundant rainfall and high relative humidity. To date, Argentina has not established DON tolerance limits. Objective: To validate a method using GC with electron capture detector (GC-ECD) and to provide evidence of DON contamination in Argentinean commercial wheat flour. Results: A total of 34 different flour samples were analyzed obtaining 91.2% of incidence with a mean level of 243 µg/kg and a median level of 165 µg/kg. The method showed acceptable LOD (24 µg/kg) and LOQ (79 µg/kg), relative SD (RSD) of the intermediate precision (RSD = 5.98%), recovery (89.3%) and uncertainty (14%). Conclusions: The method was successfully validated according to the studied parameters. Incidence results for DON contamination are low and in accordance with previous studies for years with low FHB incidence in wheat.

Evaluation of the TLC quantification method and occurrence of deoxynivalenol in wheat flour of southern Brazil

ABSTRACTThe study evaluated a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method for use with a TLC quantification procedure for deoxynivalenol (DON). It also surveyed DON occurrence in wheat flour from the southern region of Brazil. Forty-eight wheat flour samples were analysed, divided into 2 different harvest lots, each consisting of 24 different brands. The detection and quantification limits of the method were 30 and 100 ng of DON on the TLC plate. The various concentrations of DON presented high linearity (R2 = 0.99). A negative matrix effect (−28%) of the wheat flour was verified, with suppression of the chromatographic signal of DON, and 80.2–105.4% recovery. The TLC method was reliable for DON evaluation, with a coefficient of variation of less than 10%. High-performance liquid chromatography of lot 2 samples confirmed the presence of DON in all samples identified DON-positive by the TLC technique. Of the 48 wheat flour samples in lots 1 and 2 analysed by TLC, 33.3 and 45.8% of the samples respectively were above the Brazilian legislation limit. Correlations were observed between the water activity and DON content, and between the fungal count and moisture content of the wheat flours.

Occurrence of deoxynivalenol in wheat flour, instant noodle and biscuits commercialised in Brazil

ABSTRACTA total of 134 samples, consisting of 58 wheat flour, 40 instant noodle and 36 biscuits, were analysed for the presence of deoxynivalenol (DON). The samples were obtained from retail markets of the city of São Paulo during the period 2010–2014. DON was determined by high performance liquid chromatography with ultraviolet detection and immunoaffinity sample clean-up. Method validation followed international guidelines. The LOD and LOQ were 60 and 200 µg kg−1, respectively, considering the three different types of samples analysed. The lowest recovery found in this study was 91.8% with RSD 4.5% for instant noodles. DON was detected in 91.4%, 97.5% and 97.2% of samples wheat flour, instant noodles and biscuits, respectively, resulting in a total of 94.8% with levels ranging from LOD to 1720.0 µg kg−1.

Electrochemiluminescence modified electrodes based on RuSi@Ru(bpy)3(2+) loaded with gold functioned nanoporous CO/Co3O4 for detection of mycotoxin deoxynivalenol.

Nanoporous cobalt (NPCo) with three-dimensional network nanostructure was obtained by selectively dealloying Al from CoAl alloy in a mild alkaline solution. Co3O4 grew further on the surface of NPCo and then NPCo/Co3O4 was obtained. Gold nanoparticles functionalized NPCo/Co3O4 (NPCo/Co3O4-Au) was used to fabricate electrochemiluminescence (ECL) modified electrodes for detecting mycotoxin deoxynivalenol (DON). In addition the introduction of AuNPs enhanced the conductivity, and NPCo/Co3O4-Au exhibited excellent catalytic properties for the luminescence of RuSi@Ru(bpy)3(2+). The fabricated ECL modified electrodes exhibited a high activity for DON in a wide linear range from 5 pg/mL to 100 ng/mL with a low detection limit of 1 pg/mL. The NPCo/Co3O4-Au based ECL modified electrodes displayed excellent stability and reproducibility, and successfully achieved the detection of DON in wheat flour with desirable results as well. The NPCo/Co3O4-Au possesses great application potential for ECL modified electrodes with sample detection, unique catalytic activity, and high structure stability.

Monitoring levels of deoxynivalenol in wheat flour of Brazilian varieties

Deoxynivalenol (DON) is a mycotoxin produced by Fusarium graminearum and its intake represents a severe risk to human and animal health. The objective of this study was to evaluate levels of DON in wheat (Triticum aestivum L.) flour from two representative locations of south Brazil. Experiments were carried out in Pato Branco (Parana) and Coxilha (Rio Grande do Sul) in a randomized complete block design with three replicates. Levels of DON were measured by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS/MS). This mycotoxin was detected in 97% of samples, ranging from 200 to 4140 u,g kg-1. Only 17% of samples presented DON beyond of the maximum allowed by the Brazilian Health Surveillance Agency up to the year 2012; even though, Fusarium head blight (FHB) epidemics were slight low in the growing season that the study was performed. According to our knowledge, this is the first report showing genetic variability of Brazilian cultivars to DON contamination and some genotypes have potential to be exploited as a source of low accumulation of this toxin.

Magnetic nanoparticle solid phase extraction-HPLC-UV for determination of deoxynivalenol in wheat flour

Deoxynivalenol has been associated with human gastroenteritis and its presence in foods can cause clinical or subclinical manifestations in humans and animals.

Detection of deoxynivalenol in wheat flour using fluorescence fingerprint

This study focused on using fluorescence fingerprint (FF) to detect DON non-destructively. The fluorescence fingerprint is also called excitation-emission matrix, which consists of an excitation wavelength axis, an emission wavelength axis, and a fluorescence intensity axis. It is acquired by measuring the fluorescence intensity of a sample at consecutive excitation and emission wavelengths. The samples were wheat grains artificially contaminated with 4 levels of DON. They were crushed into flour. FF measurement was made by a fluorescence spectrometer using a powder cell. Both excitation wavelength and emission wavelength ranges were from 200 to 900nm at each 10nm interval. Three analyses for FF data were carried out to confirm the possibility of DON detection. Principal component analysis (PCA) was applied to the FF data. The result of PCA indicated that PC2 could become an index of DON contamination degree. Discriminant analysis was also carried out to the same data. Canonical 1 can discriminate the samples based on the DON contamination. Partial Least Squares Regression was applied to the quantitative sample data. Half of data set was used for the calibration and the rest was used for validation. R2 for calibration and validation set were 0.990 and 0.983, respectively. As a result, fluorescence fingerprint has possibility to become practical technique for screening of DON contamination.

蛍光指紋による小麦粉中のデオキシニバレノールの非破壊計測

蛍光指紋による小麦粉中のデオキシニバレノールの非破壊計測

Optimisation of the determination of deoxynivalenol in wheat flour by HPLC and a comparison of four clean-up procedures

The determination of deoxynivalenol (DON) in wheat flour by liquid chromatography with photodiode array (PDA) detection was optimised. Response surface methodology (RSM) was used to determine the optimum chromatographic conditions for the determination of DON. The influence of three variables, acetonitrile (ACN) volume in mobile phase (9.5–24.5, v/v), flow rate (0.5–1.5 ml min−1) and wavelength (215–221 nm) on DON peak area was evaluated. The best separation was achieved using a symmetry column (150 × 3.9 mm; particle size 5 µm) by isocratic elution (1.0 ml min−1) and a mobile phase consisting of ACN/water in the ratio 17 : 83 (v/v). UV detection was performed at 218 nm. Linear calibration curves were constructed in the concentration range 1–1000 ng ml−1. The detection limit measured as the signal-to-noise ratio (3 : 1) was 0.03 ng ml−1. RSM results showed that the experimental data could be adequately fitted to a second-order polynomial model with multiple regression coefficients (R 2) of 0.968. The efficiency of four clean-up procedures for wheat flour extract was compared. Recovery of DON using a Mycosep #225 column was highest with a value of 99%, while that of Mycosep #227 was 65%. In contrast, DON recovery using immunoaffinity columns (IAC) and an Oasis® HLB column was only 53 and 42%, respectively. The trueness of the method using the Mycosep #225 column was established with a certified reference material CRM 379. The result obtained from three replicates was 0.66 ± 0.04 µg g−1 and the certified value was 0.67 µg g−1.

Untersuchungen zu DON-Gehalten in Getreideerzeugnissen aus dem deutschen Einzelhandel im Jahr 2006

Samples of soft wheat flour (n=78), durum wheat semolina (n=6), and pasta (made from durum wheat, n=49) were purchased in January-April 2006 from retail outlets in Hesse, Germany. Samples were analysed for deoxynivalenol (DON) by enzyme immunoassay. The detection limit of the method was 10 μg/kg, with recoveries of 81–85% (RSDr: 12–17%). DON was detected in 84% of all samples, but the contamination level was low. Median/maximum values for DON in wheat flour, wheat semolina, and pasta were 28μg/kg/217 μg/kg, 38μg/kg/203 μg/kg, and 24μg/kg/119 μg/kg, respectively. Compared with results obtained from previous years, significantly lower DON levels were observed in these commodities.

A research of deoxynivalenol in wheat flour traded in portugal: [formula omitted], M.C. Batoréu and M.I. Felgueiras Toxicology Department of Faculty of Pharmacy of University of Lisbon and INETI/IBQTA/DTIA. Av. Forças Armadas, 1699 Lisboa Codex, Portugal

A research of deoxynivalenol in wheat flour traded in portugal: [formula omitted], M.C. Batoréu and M.I. Felgueiras Toxicology Department of Faculty of Pharmacy of University of Lisbon and INETI/IBQTA/DTIA. Av. Forças Armadas, 1699 Lisboa Codex, Portugal