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1.
A new method for the simultaneous quantification of 12 mycotoxins was developed and optimized using reverse phase high performance liquid chromatography (RP-HPLC) with a photodiode array (PDA) and fluorescence detector (FLD), a photochemical reactor for enhanced detection (PHRED) and post-column derivatization. The mycotoxins included aflatoxins (AFB1, AFB2, AFG1, and AFG2), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB1, FB2, and FB3), T-2 and HT-2 toxins. A double sample extraction with a phosphate-buffered saline solution (PBS) and methanol was used for co-extraction of mycotoxins, and a multifunctional immunoaffinity column was used for cleanup. Optimum conditions for separation of the mycotoxins were obtained to separate 12 mycotoxins in FLD and PDA chromatograms with a high resolution. The method gave recoveries in the range 72–111% when applied to spiked corn samples. The limits of detection (LOD) were 0.025?ng/g for AFB1 and AFG1, 0.012?ng/g for AFB2 and AFG2, 0.2?ng/g for OTA, 1.5?ng/g for ZEA, 6.2?ng/g for FB1, FB3 and HT-2 toxin, 9.4?ng/g for FB2 and T-2 toxin, and 18.7?ng/g for DON. In addition, the limits of quantification (LOQ) ranged from 0.04?ng/g for AFB2 and AFG2 to 62?ng/g for DON. The method was successfully applied to the determination of these mycotoxins in 45 cereal samples obtained from the Malaysian market. The results indicated that the method can be applied for the multi-mycotoxin determination of cereals.  相似文献   

2.
A liquid chromatography tandem mass spectrometry (LC–MS/MS) method is described for simultaneous determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB1 and FB2), T2 and HT2-toxin in cereals. One-step extraction using solvent mixtures of acetonitrile:water:acetic acid (79:20:1) without any clean-up was employed for extraction of these mycotoxins from cereals. The mean recoveries of mycotoxins in spiked cereals ranged from 76.8% to 108.4%. Limits of detection (LOD) and quantification (LOQ) ranged 0.01–20 and 0.02–40 ng/g, respectively. The developed method has been applied for the determination of mycotoxins in 100 cereal samples collected from Malaysian markets. A total of 77 cereal samples (77%) contaminated with at least one of these mycotoxins. Occurrence of mycotoxins in commercial cereal samples were 70%, 40%, 25%, 36%, 19%, 13%, 16, and 16% for aflatoxins, OTA, ZEA, DON, FB1, FB2, T2 and HT2-toxin, respectively. The results demonstrated that the procedure was suitable for the determination of mycotoxins in cereals and could be implemented for the routine analysis.  相似文献   

3.
ABSTRACT

A total of 576 samples marketed in China, including maize, maize flour, maize grits and maize meal, was determined for the simultaneous presence of 12 mycotoxins (FB1, FB2, FB3, DON, 3-DON, 15-DON, ZEN, AFB1, AFB2, AFG1, AFG2 and OTA) using a validated UPLC-MS/MS for multi-mycotoxin method. DON were the most widespread mycotoxins (63%), followed by FB1 (57%) and ZEN (46%). 78% of the samples was contaminated with at least one of these mycotoxins. Risk assessment indicated that maize and maize-derived food intake does not pose a potential risk for general adult population with respect to individual mycotoxin. However, two or more mycotoxins were detected in 60% of all samples, and a combination of up to seven different mycotoxins was found. A particular attention should be paid to the combined exposure of mycotoxins, in this cases the estimated daily intake might increase greatly due to the high frequency of co-occurrence.  相似文献   

4.
A reliable and sensitive liquid chromatography/tandem mass spectrometry (LC‐MS/MS) method was developed for the simultaneous determination of aflatoxins (AFB1, AFB2, AFG1, and AFG2), ochratoxin A (OTA), deoxynivalenol (DON), zearalenone (ZEA), fumonisin B1 (FB1), and T2‐toxin in maize. The samples were first extracted using acetonitrile: water: acetic acid (79 : 20 : 1), and then further cleaned‐up using OASIS HLB cartridge. Optimum conditions for the extraction and chromatographic separation were investigated. The mean recoveries of mycotoxins in spiked maize ranged from 68.3% to 94.3%. Limits of detection and quantification ranged from 0.01 to 0.64 μg/kg and from 0.03 to 2.12 μg/kg, respectively. The LC‐MS/MS method has also been successfully applied to 60 maize samples, which were collected from Shaanxi Province of China. Twenty‐four of the total 60 samples (40%) were contaminated with at least 1 of these 9 mycotoxins. Occurrence of mycotoxins were 6.7%, 1.7%, 3.3%, 6.7%, 1.7%, 23.3%, and 3.3% for AFB1, AFB2, OTA, ZEA, DON, FB1, and T2‐toxin, respectively. The results demonstrated that the procedure was suitable for the simultaneous determination of these mycotoxins in maize matrix.  相似文献   

5.
Mycotoxins are secondary metabolites produced by fungi, such as Fusarium, Penicillium, and Aspergillus, which are toxic to humans with high risk factors and pose a significant threat to human health. This study was focused mostly on well-known mycotoxins, such as aflatoxins (AFB1, AFB2, AFG1 and AFG2), fumonisin (FB1, FB2), deoxynivalenol (DON), zearalenone (ZON), ochratoxin A, T-2 and HT-2, in grains. The multi-mycotoxin methods developed in this study utilise an analysis of mycotoxin through liquid chromatography tandem mass spectrometry (LC-MS/MS), which can significantly improve sample analysis efficiency. The Myco6in1? immunoaffinity column was used for purification to reduce interference from the substrate. Gradient separation to obtain the best peak shift was conducted using solvent with 0.1 % formic acid in deionised water and methanol, and gradient separation was performed on an ACQUITY BEH C18 column chromatograph. The recovery rate test for each toxin using substrates such as rice, peanut, wheat and maize mostly indicated good average recovery rates between 70 % and 120 % and the coefficient of variation mostly under 15 %. The limits of quantification (LOQ) identified by this method are less than 5 ng/g in most toxins, except for 20 ng/g in FB1and FB2. This method can rapidly and simultaneously analyse 11 mycotoxins in 9 min. It can be applied for the practical examination of mycotoxins in food to protect public health.  相似文献   

6.
Palm kernel cake (PKC) is a useful source of protein and energy for livestock. Recently, it has been used as an ingredient in poultry feed. Mycotoxin contamination of PKC due to inappropriate handling during production and storage has increased public concern about economic losses and health risks for poultry and humans. This concern has accentuated the need for the evaluation of mycotoxins in PKC. Furthermore, a method for quantifying mycotoxins in PKC has so far not been established. The aims of this study were therefore (1) to develop a method for the simultaneous determination of mycotoxins in PKC and (2) to validate and verify the method. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method using an electrospray ionisation interface (ESI) in both positive- and negative-ion modes was developed for the simultaneous determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), zearalenone (ZEA), deoxynivalenol (DON), fumonisins (FB1 and FB2), T-2 and HT-2 toxin in PKC. An optimum method using a 0.2 ml min–1 flow rate, 0.2% formic acid in aqueous phase, 10% organic phase at the beginning and 90% organic phase at the end of the gradient was achieved. The extraction of mycotoxins was performed using a solvent mixture of acetonitrile–water–formic acid (79:20:1, v/v) without further clean-up. The mean recoveries of mycotoxins in spiked PKC samples ranged from 81% to 112%. Limits of detection (LODs) and limits of quantification (LOQs) for mycotoxin standards and PKC samples ranged from 0.02 to 17.5 μg kg?1 and from 0.06 to 58.0 μg kg?1, respectively. Finally, the newly developed method was successfully applied to PKC samples. The results illustrated the fact that the method is efficient and accurate for the simultaneous multi-mycotoxin determination in PKC, which can be ideal for routine analysis.  相似文献   

7.
Fumonisins B1, B2 and B3 (FB1, FB2 and FB3) and aflatoxins B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2) are both major mycotoxins of food concern, because of their wide range of concentration and possible co-occurrence. Therefore, a contamination survey in corn and wheat flour by liquid chromatography–tandem mass spectrometry was carried out. Quantification of fumonisins and aflatoxins was based on internal calibration (by the use of 13C34-fumonisin) and external calibration, respectively. Fumonisins were detected in 95% of corn samples and in 7% of wheat flour samples, with the mean level (FB1?+?FB2?+?FB3) of 441?µg?kg?1 and 0.09?µg?kg?1, respectively. Low levels of aflatoxins were detected in 37% of the samples with a mean level (B1?+?B2?+?G1?+?G2) of 0.12?µg?kg?1. Fumonisins and aflatoxins were not detected in 29% of the samples analysed. Simultaneous occurrence of fumonisins and aflatoxins was observed in 12% of samples.  相似文献   

8.
Beer is an alcoholic beverage made from a cereal grain extract and is widely consumed in sub‐Saharan Africa and the world at large. However, beer consumption could expose consumers to mycotoxins. In this review, we appraised the different mycotoxins associated with beer contamination, elucidating their structures and incidence in cereals involved in beer production. The common mycotoxins that are found within the brewing process are reviewed. These include aflatoxin B1 (AFB1), fumonisin (FB), ochratoxin A (OTA), zearalenone (ZEA) and deoxynivalenol (DON), which are the prime contaminants in beer produced in sub‐Saharan Africa. Residual levels of <20% of AFB1, OTA and FB2 together with the transformation of ZEA (into a less toxic compound β‐zearalenol) can be achieved during the production of beers originating from Europe/America, while >50% of DON and higher ratios of FB1 can be recovered in finished beer. Adsorption is the major means of mycotoxin removal during beer production. In contrast, traditional African beer processes show no significant efficient removal of mycotoxins. This is because the prevailing environmental conditions during beer production are favourable to mycotoxigenic fungal proliferation. This subsequently leads to relatively high concentration of mycotoxins in freshly processed beer, with a possible increase during the beer shelf‐life owing to the absence of appropriate microbial stabilisation treatments in the finished processed beer. © 2019 The Institute of Brewing & Distilling  相似文献   

9.
The natural occurrence of ochratoxin A, ochratoxin B, aflatoxin B1, aflatoxin B2, aflatoxin G1 and aflatoxin G2 (OTA, OTB, AFB1, AFB2, AFG1, AFG2) in red wines was investigated by HPLC/FLD after immunoaffinity column clean-up in 57 market samples produced in Sicily (Italy). The results showed a very low incidence of these mycotoxins in analysed samples, confirming the high degree of quality and safety of Sicilian red wines. The results indicated 71.9% and 64.9% positive samples for OTA and OTB respectively, with an average level of 0.13 μg l–1, well below the European maximum permitted levels (MLs). The aflatoxin most frequently detected in the samples was AFG1, present in 57.9% of samples, while the other aflatoxins were rarely present. Recovery experiments were carried out on eight mycotoxin-free red wines spiked with OTA, OTB, AFB1, AFB2, AFG1 and AFG2 at two different levels. The limits of detection (LODs) in wines were 0.02 µg l–1 for OTA, 0.04 µg l–1 for OTB, 0.03 µg l–1 for AFG1, AFG2 and AFB2, and 0.05 µg l–1 for AFB1. A good correlation was found, with good performances in term of precision for the method.  相似文献   

10.
The objective of this study was to determine the distribution of an economically important class of mycotoxins, the aflatoxins, in rice milling fractions. Rice plants grown under field production conditions are frequently infected with types of pathogenic fungi that produce toxic metabolites (mycotoxins). Paddy (seeds) rice from healthy plants in the field was collected and stored on a farm under humid, poorly ventilated conditions. Samples were milled into four fractions (hulls, brown rice, bran and white rice) and analysed for aflatoxins (B1, B2, G1 and G2) using a validated method. Rice fractions from healthy plants, which contained low levels of aflatoxins (less than 1?µg?kg?1), were used to determine the efficiency of the extraction method. Seeds stored under poor conditions were found to be contaminated with aflatoxins B1 and B2 as were the fractions. The sums of AFB1 and AFB2 in stored paddy rice, hulls, brown rice, bran and white rice were 141, 39, 158, 367 and 56?µg?kg?1, respectively. The ratio of aflatoxin B1 and B2 was about 10?:?1. AFG1 and AFG2 were less than 1?µg?kg?1. Thus, brown rice contained 92.9% of the aflatoxins in paddy rice, whereas white rice contained only 27.9%.  相似文献   

11.
A survey of 11 mycotoxins in 348 wheat flour samples marketed in Hebei province of China were analysed by liquid chromatography-tandem mass spectrometry, was carried out. The selected mycotoxins consisted of four aflatoxins (AFs: AFB1, AFB2, AFG1 and AFG2) and seven Fusarium toxins, i.e. deoxynivalenol (DON), nivalenol, 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol, zearalenone, Fusarenon-X and deoxynivalenol-3-glucoside. Results indicated that most of the wheat samples analysed were contaminated with mycotoxins. Wheat was most susceptible to DON (91.4% contamination), with a mean level of 240 μg kg?1. On average the probable daily intake (PDI, expressed as µg kg?1 body weight day?1) of mycotoxins was within the provisional maximum tolerable daily intake (PMTDI, 2.0 µg kg?1 of body weight day?1) as set by the Joint FAO/WHO Expert Committee on Food Additives. Nevertheless, exposure assessment revealed that the maximum PDI of mycotoxins was 4.06 µg kg?1 body weight day?1, which was twice the PMTDI value. Thus, consistent monitoring is recommended, as to keep the contamination level under control.  相似文献   

12.
A simple method for the reduction of aflatoxins B1 (AFB1), B2 (AFB2), G1 (AFG1), G2 (AFG2) and ochratoxin A (OTA) in white pepper was studied. Response surface methodology (RSM) was applied to determine the effect of four variables, which included time (20–60?min), temperature (30–70°C), calcium hydroxide (Ca(OH)2) (0–1%) and hydrogen peroxide (H2O2) (1–3%) during the washing step of white pepper. The efficacy of the method was evaluated by the determination of mycotoxins by HPLC with fluorescence detection (FD). Statistical analysis showed that the experimental data could be adequately fitted into a second-order polynomial model, with a multiple regression coefficient (R 2) in the range of 0.805–0.907 for AFG2 and AFG1, respectively. The optimal condition was 57.8?min, 62.0°C, of 0.6% (w/v) and 2.8% (v/v) for time, temperature, Ca(OH)2 and H2O2 respectively. By applying the optimum condition, the mycotoxins reduction was found to be in the range of 68.5–100% for AFB2 and AFG1 respectively.  相似文献   

13.
Seventy five samples of two popular lager beers, namely Pilsner and Tusker were randomly collected from the city of Nairobi and the surrounding satellite towns in Kenya. The samples were analyzed for the presence of 4 mycotoxins, namely, deoxynivalenol (DON), fumonisin B1 (FB1), zearalenone (ZEA), and aflatoxin B1 (AFB1), by the competitive enzyme linked immunosorbent assay (ELISA) technique. The incidences of DON and ZEA were 100% in both brands, while for FB1 the incidence was 72%, with incidences in Tusker (76.9%) being significantly higher than in Pilsner (66.7%) (p = 0.00). The mean values for contamination were 3.29 and 3.57 ng/mL for DON, 0.28 and 0.32 ng/mL for FB1 and 7.84 and 8.50 pg/ml for ZEA in Tusker and Pilsner brands respectively. A positive occurrence association was found between DON and FB1 and DON and ZEA, an indication of their common source from Fusarium sp. The results suggest low levels and safe exposure to consumers of Kenyan lager beers with Fusarium mycotoxins.  相似文献   

14.
为探明西藏高原粮油作物曲霉菌污染状况及黄曲霉菌产毒能力,连续5年对西藏青稞、小麦、花生3种作物中曲霉菌污染情况进行分析,并对其分离到的黄曲霉菌株开展产毒力研究,结果表明,204份样品中,共分离出15种曲霉菌,曲霉菌污染率呈花生>青稞>小麦。青稞、小麦中曲霉属优势种均为黑曲霉(Aspergillus niger),真菌毒素主要为杂色曲霉毒素和赭曲霉毒素;花生优势种为黄曲霉(A.flavus);仅受黄曲霉毒素污染。来源于不同作物的黄曲霉菌,其产毒类型也有差异,麦类作物产毒菌株以产黄曲霉毒素B1(AFB1)、黄曲霉毒素B2(AFB2)为主;花生产毒菌株以产AFB1、AFB2、AFG1、AFG2为主。  相似文献   

15.
ABSTRACT: The objective of this work was to determine the reduction of aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1), and G2 (AFG2) as a function of initial moisture content of samples (24%, 27%, and 30%), barrel temperature (140, 170, and 200 °C), and residence time (30 to 70 s) when artificially contaminated rice meal was extrusion‐cooked. Extruded and unextruded samples were analyzed by high‐performance liquid chromatography (HPLC). Extrusion‐cooking was observed to reduce aflatoxin (AF) content, which ranged from 51% to 95% depending on the type of AF and the studied variables. Only in the case of AFG2 was it found that the higher the temperature, the higher the moisture content, and the longer the residence time, the greater the reduction. Moisture content had a significant influence on reducing AFB2, AFG1, and AFG2 whereas it was not a significant factor affecting the levels of AFB1. Regardless of the type of AF, the lowest reductions were achieved at a temperature of 140 °C. Even though theoretically greater losses would be expected at highest temperature, AFB1 and AFB2 were more reduced by 170 °C than by 200 °C while AFG1 reductions were not statistically different when processing at 170 °C and 200 °C. The decrease of AF followed 1st‐order kinetics; the fastest treatment in reducing AF was that at 200 °C when samples containing AFG2 were wetted to 24% and when samples containing AFB1, AFB2, and AFG1 were hydrated to 27%. By contrast, the slowest treatments were observed at a barrel temperature of 140 °C.  相似文献   

16.
Brazil is the sixth largest producer of cocoa beans in the world, after Côte d’Ivoire, Ghana, Indonesia, Nigeria and Cameroon. The southern region of Bahia stands out as the country’s largest producer, accounting for approximately 60% of production. Due to damage caused by infestation of the cocoa crop with the fungus Moniliophthora perniciosa, which causes ‘witch’s broom disease’, research in cocoa beans has led to the cloning of species that are resistant to the disease; however, there is little information about the development of other fungal genera in these clones, such as Aspergillus, which do not represent a phytopathogenicity problem but can grow during the pre-processing of cocoa beans and produce mycotoxins. Thus, the aim of this work was to determine the presence of aflatoxin (AF) and ochratoxin A (OTA) in cocoa clones developed in Brazil. Aflatoxin and ochratoxin A contamination were determined in 130 samples from 13 cocoa clones grown in the south of Bahia by ultra-performance liquid chromatography with a fluorescence detector. The method was evaluated for limit of detection (LOD) (0.05–0.90 μg kg?1), limit of quantification (0.10–2.50 μg kg?1) and recovery (RSD) (89.40–95.80%) for AFB1, AFB2, AFG1, AFG2 and OTA. Aflatoxin contamination was detected in 38% of the samples in the range of ?1, with AFB1 in 25% of the total samples, whereas ochratoxin A was positive in 18% of the samples in the range of ?1.  相似文献   

17.
A sensitive and selective liquid chromatography–triple quadrupole–tandem mass spectrometry (LC–ESI–MS–MS) method was developed for the routine analysis of aflatoxins (AFB1, AFB2, AFG1 and AFG2) and ochratoxin A (OTA) in tiger nuts and tiger-nut beverage (horchata). A matrix solid phase dispersion was adapted to eliminate lipidic interferences. The solid support was C18, while the elution solvent was acetonitrile. Mean recoveries obtained at two fortification levels were 72–83% and 71–81% for horchata and tiger nut respectively with relative standard deviations (RSDs) <13% and 15% respectively. The LC–MS–MS method allowed quantification and identification at low levels in two matrices. The method was applied for the routine analysis of tiger-nuts and horchata samples collected from different supermarkets of Valencia (Spain) during one year (March 2009–March 2010). A total of 238 samples were analysed and 32 samples were found positives for OTA, AFB1, AFB2 and AFG2.  相似文献   

18.
Naturally occurring mycotoxins are responsible for a wide array of adverse health effects. The measurement of urinary mycotoxin levels is a useful means of assessing an individual's exposure, but the development of sensitive and accurate analytical methods for detecting mycotoxins and their metabolites in urine samples is challenging. Urinary mycotoxins are present in low pg ml–1 concentrations, and the chromatographic identification of their metabolites can be obscured by other endogenous metabolites. We developed an analytical method focused on the selection of two appropriate multiple-reaction monitoring transition for unambiguous identification and quantification of carcinogenic aflatoxin M1 (AFM1), ochratoxin A (OTA) and fumonisin B1, B2 (FB1, FB2) in urine samples from a small volunteer group in a pilot study. AFM1, OTA, FB1 and FB2 were concentrated selectively, interfering substances were removed using an immunoaffinity column (IAC), and mycotoxins were measured using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in combination with a stable-isotope standard-dilution assay (SIDA). The method was sensitive enough to measure mycotoxins and their metabolites at pg ml–1 levels in urine. The combination of LC-MS/MS and SIDA was critical to distinguishing pseudo-OTα interference from genuine OTα. Twelve urine samples contained OTA ranging from 0.013 to 0.093 ng ml?1 (mean = 0.031 ng ml?1). AFM1 were detected in one sample at a 0.002 ng ml?1 level, while FB1 and FB2 were undetectable in all 12 samples. None of the samples in this pilot study contained a detectable level of OTα, despite the presence of OTA, and this may suggest the need for further epidemiological investigation of OTA exposure in the Korean population.  相似文献   

19.
A total of 57 samples of corn and corn‐based products collected from various districts of Egypt were analyzed for Fusarium mycotoxins (T‐2, diacetoxyscripenol (DAS( deoxynivalenol (DON) and fumonisin B1 (FB1) and aflatoxins. FB1 was detected in about 80%, 53.85%, 33.3%, and 28.57% of yellow corn, corn meal, white corn, and popcorn samples, respectively. The levels of FB1 ranged from 10 to 780 μg/kg. T‐2 and DAS were detected in 5% and 10% of yellow corn samples, respectively, and DON was detected in white corn and popcorn samples at levels of 28.8 and 10.1 μg/kg, respectively. Starch samples were found to be free from Fusarium mycotoxins. Baking balady bread at 450°C/min reduced FB1 to 72.4% while baking Franco bread at 250°C/20 min reduced FB1 to 57.4%. Boiling of macaroni and corn in water completely removed FB1 from contaminated samples. On the other side, corn flakes samples were found to be contaminated with aflatoxins B1 and G1 at levels ranging from 6 to 10 ppm, whereas 2.9% of samples were contaminated with aflatoxin B1 > 35 ppm and G1 > 16 ppm.  相似文献   

20.
Analysis of aflatoxin B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2) in 76 edible oil samples (peanut oil, soybean oil, corn embryo oil and blended oil) was performed by liquid chromatography–tandem mass spectrometry (LC–MS/MS). The oils were sampled from three areas (Shijiazhuang, Baoding and Tangshan) of Hebei Province of China. AFB1 was detected in 22 samples representing 28.9%, followed by AFB2 (7.89%) and AFG1 (3.95%), while no AFG2 contamination was detected in any samples. AFB1 levels in oil samples ranged 0.14–2.72?µg?kg?1 and AFB2 ranged 0.15–0.36?µg?kg?1, while lower levels of 0.01–0.02?µg?kg?1 for AFG1 were recorded. The paper is part of an on-going investigation of aflatoxin contamination in Chinese edible oils.  相似文献   

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