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1.
Sorghum samples (n = 60) from Tunisian markets were analysed for the occurrence of 22 of both traditional and emerging mycotoxins. Samples were extracted with a QuEChERS-like method and mycotoxins were detected by LC-MS/MS. This method was validated and adequate analytical parameters were obtained. All samples had contamination with mycotoxins and several samples had higher contamination levels than European Union legislative limits (MLs). The most frequently found mycotoxins were ENB (100%), OTA (98%), ENA1 (63%), ENB1 (56%), BEA (48%), AFB1 (38%) and STG (33%). Mean contaminations were 30.7, 1.93, 33.2, 51.0, 15.4, 1.49 and 20.5 µg kg–1, respectively. While two samples were contaminated with FB2 and FB3 at mean values of 16.2 and 45.9 µg kg–1, respectively, one sample was contaminated with AFB2 and ZEA at levels of 0.82 and 45.0 µg kg–1, respectively. The results were used to estimate the daily intake of mycotoxins through sorghum consumption with regard to normal consumers (low-risk population) and high consumers such as babies (high-risk consumers) who are facing an alarming situation.  相似文献   

2.
An ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) multi-mycotoxin analytical method was developed to simultaneously identify and quantify 20 mycotoxins in grass silages, inclusive of mycotoxins that are currently regulated in European Union feeds. Extraction of mycotoxins from dried grass silages was performed using of a modified QuEChERS extraction employing an acidified aqueous extraction (0.1 N HCl) with no further clean-up. Following chromatographic separation, analytes were detected using a fast polarity-switching MS/MS method that allowed both positive and negative ions to be analysed from a single injection, thus the reducing time and cost of analysis. The limits of detection and quantification ranged between 3 µg kg–1 DM (aflatoxin B1, beauvericin and enniatin A and A1) and 200 µg kg–1 DM (deoxynivalenol), and between 10 µg kg–1 DM (aflatoxin B1, beauvericin and enniatin A1) and 500 µg kg–1 DM (deoxynivalenol), respectively. Inter-assay accuracy and precision ranged between 90% and 107% and between 3.9% and 15.0% CV, respectively. The accuracy of the method was assessed through the application to a range of incurred samples in an inter-laboratory study.  相似文献   

3.
The occurrence of the emerging mycotoxins enniatins (ENNs) and beauvericin (BEA) has been reported in Fusarium-infected cereals. To study the effect of sourdough processing and baking on ENN B, ENN B1, and BEA concentrations, a recently developed stable isotope dilution assay for these mycotoxins was used. After milling of wheat and rye grains naturally contaminated with ENN B and ENN B1, approximately 70–82 % of the two ENNs were found in the bran fraction and the rest remained in flour. BEA was added to flour before sourdough fermentation. In an experiment on a microscale, dough was fermented for 24 h at 30 or 40 °C, which reduced part of the ENNs and BEA in particular at 40 °C. On a standard scale, mixing, resting, and proofing of the bread dough resulted in 13–19 % reduction of the ENNs compared with flour, but in no significant change of BEA. The final baking at 200 °C for 25 min led to a further decrease of the ENNs and BEA, ranging from 9 to 28 % compared with fermented dough. In case of rye sourdough bread, greater reductions of ENNs were found in crust than in crumb. For both wheat and rye flours, overall 25–41 % of ENN B, ENN B1, and BEA were reduced during the whole sourdough bread-making process.  相似文献   

4.
ABSTRACT

This study determined the levels of pyrrolizidine alkaloids (PAs), including their respective N-oxides, in foodstuffs available in Hong Kong by liquid chromatography-electrospray ionisation tandem mass spectrometry. A total of 234 samples (48 food items) were collected randomly from a local market and analysed. About 50% of samples were found to contain detectable amount of PAs. Amongst the 48 food items, PAs were not detected in 11 food items, including barley flour, beef, cattle liver, pork, pig liver, chicken meat, chicken liver, milk, non-fermented tea, Melissa tea and linden tea. For those found to contain detectable PAs, the summed PA content ranged up to 11,000 µg kg?1. The highest sum of PA content among the 37 food items calculated with lower bound was cumin seed, then followed by oregano, tarragon and herbs de Provence with ranges of 2.5–11,000, 1.5–5100, 8.0–3300 and 18–1300 µg kg?1 respectively. Among the samples, the highest sum of PA content was detected in a cumin seed sample (11,000 µg kg?1), followed by an oregano (5100 µg kg?1), a tarragon (3300 µg kg?1) and a herbs de Provence (1300 µg kg?1). In general, the results of this study agreed well with other published results in peer-reviewed journals, except that the total PAs in honey and specific tea infusion in this study were comparatively lower.  相似文献   

5.
Dietary exposure of Hong Kong adults to mycotoxins and their metabolites including aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FNs), deoxynivalenol (DON), acetyldeoxynivalenols (AcDONs) and zearalenone (ZEA) was estimated using the Total Diet Study (TDS) approach to assess the associated health risk to the local people. Sixty commonly consumed food items, collected in four seasons, were sampled and prepared as consumed. These mycotoxins were primarily found at low levels. The highest mean levels (upper bound) were: AFs, 1.50 µg kg1 in legumes, nuts and seed; OTA, 0.22 µg kg1 in sugars and confectionery; FNs, 9.76 µg kg1 in cereals and their products; DON and AcDONs, 33.1 µg kg1 in cereals and their products; and ZEA, 53.8 µg kg1 in fats and oils. The estimated dietary exposures of Hong Kong adults to the mycotoxins analysed were well below the respective health-based guidance values, where available. For AFs, the upper-bound exposure for high consumers is 0.0049 µg kg bw1 day1, which was estimated to contribute to about 7.7 (< 1%) of liver cancer cases when compared with 1222 liver cancer cases per year in Hong Kong. The percentage contributions of the estimated 95th percentile dietary exposures (lower and upper bound) to the health-based guidance values of individual mycotoxins were: ochratoxin A, 3.6–9.2%; fumonisins, 0.04–8.5%; deoxynivalenol and acetyldeoxynivalenols, 21.7–28.2%; and zearalenone 3.3–34.5%. The findings indicate that dietary exposures to all the mycotoxins analysed in this study were unlikely to pose an unacceptable health risk to the Hong Kong population.  相似文献   

6.
A total of 64 samples of sorghum (37 Tunisian sorghum samples and 27 Egyptian sorghum samples) were collected during 2011–2012 from markets in Tunisia. Samples were analysed for contamination with aflatoxin B1, ochratoxin A and zearalenone by High-Performance Liquid Chromatography Coupled with Fluorescence Detection (HPLC-FLD). Aflatoxin B1 was found in 38 samples in the range 0.03–31.7 µg kg?1. Ochratoxin A was detected in 24 samples with concentrations ranging from 1.04 to 27.8 µg kg?1. Zearalenone was detected in 21 samples and the concentration varied between 3.7 and 64.5 µg kg?1. ANOVA analysis of the influence of the country of origin on the incidence and concentration of mycotoxins in the samples studied showed no significant difference (P > 0.05) between the two batches of samples for each of the three mycotoxins studied. The studied mycotoxins contaminate sorghum and may also co-exist because of the diversity of the mycobiota in this cereal.  相似文献   

7.
Cocoa beans are the principal raw material for chocolate manufacture. Moulds have an important place in the change in the quality of cocoa beans due to their role in the production of free fatty acids and mycotoxins, namely ochratoxin A (OTA). This study investigated the impact of the key post-harvest treatments, namely the fermentation and drying methods on OTA contamination of raw cocoa beans. Analytical methods for OTA detection were based on solid–liquid extraction, clean-up using an immunoaffinity column, and identification by reversed-phase HPLC with fluorescence detection. Of a total of 104 randomly selected cocoa samples analysed, 32% had OTA contents above 2 µg kg–1. Cocoa sourced from pods in a bad state of health had a maximum OTA content of 39.2 µg kg1, while that obtained from healthy pods recorded 11.2 µg kg–1. The production of OTA in cocoa beans increased according to the pod-opening delay and reached 39.2 µg kg–1 after an opening delay of 7 days after harvest, while 6.1 and 11.2 µg kg–1 were observed when pods were opened after 0 and 4 days. OTA production also seemed to depend considerably to the cocoa fermentation materials. When using plastic boxes for bean fermentation, the OTA production was enhanced and reached an average OTA content of about 4.9 µg kg1, while the raw cocoa treated in banana leaves and wooden boxes recorded 1.6 and 2.2 µg kg–1 on average respectively. In parallel, the OTA production was not really influenced by either the mixing or the duration of the fermentation or the drying materials.  相似文献   

8.
The aim of this study was to determine the level of bound 3-monochloropropan-1,2-diol in foodstuffs commonly consumed in Hong Kong, China, by an enzymatic hydrolysis indirect method which proved to be free from interferences. A total of 290 samples were picked up randomly from the local market and analysed. About 73% of these samples were found to contain detectable amounts of bound 3-MCPD. Amongst the 73 food items, bound 3-MCPD was not detected in 13 food items, including extra virgin olive oil, beef ball/salami, beef flank, ham/Chinese ham, nuts, seeds, soy sauce, oyster sauce, butter, yoghurt, cream, cheese and milk. For those found to contain detectable bound 3-MCPD, the content ranged up to 2500 µg kg?1. The highest mean bound 3-MCPD content among the 14 food groups was in biscuits (440 [50–860] µg kg?1), followed by fats and oils (390 [n.d.–2500] µg kg?1), snacks (270 [9–1000] µg kg?1), and Chinese pastry (270 [n.d.–1200] µg kg?1). Among the samples, the highest bound 3-MCPD content was in a grape seed oil (2500 µg kg?1), followed by a walnut flaky pastry (1200 µg kg?1) and a grilled corn (1000 µg kg?1). Basically, the results of this study agreed well with other published results in peer-reviewed journals, except for cheese, cream, ham, nuts and seeds.  相似文献   

9.
ABSTRACT

A reliable, fast and simple method using UHPLC-MS/MS was developed for the determination of aflatoxins B1 (AFB1), G1 (AFG1), B2 (AFB2) and G2 (AFG2), ochratoxin A (OTA), deoxynivalenol (DON), zearalenone (ZEA), HT-2 toxin and T-2 toxin in crude extracts of biscuits with fruit filling, cookies, dried fruits and fruit jams. The method was successfully demonstrated on 39 samples of biscuits with fruit filling, 34 cookies, 14 dried fruits and 10 fruit jams. The mycotoxins detected in biscuits samples were ZEA, OTA, T-2 and AFB1 with an average concentrations of positive samples of 2.64, 4.10, 8.13 and 1.32 µg kg?1, respectively; while the mycotoxins detected in jam samples were AFB1, OTA, T-2 and AFB2 with an average concentrations of positive samples of 2.00, 17.7, 4.37 and 1.15 µg kg?1, respectively. The results showed that the majority of samples were in compliance with relevant regulations. However in eight samples of biscuits and three samples of fig jam the contents of OTA were higher than the existing OTA limits. The combined dietary exposure of selected mycotoxins was estimated for the first time for children, adolescents and adults. The estimated combined dietary exposures were all lower than the proposed value assumed to predict a possible risk scenario.  相似文献   

10.
A simple analytical method for the determination of hydrocortisone and progesterone in bovine, swine, and chicken muscle and eggs was developed. Hydrocortisone and progesterone were extracted with acetonitrile and subsequently cleaned-up using an Oasis® HLB mini-cartridge. The method was validated in accordance with Japanese guidelines and exhibited trueness from 86.6% to 104.3% and precision (relative standard deviations (RSDs) of repeatability and within reproducibility were under 8.7% and 11.7%, respectively). The method was applied to 103 bovine muscle, 137 swine muscle, 69 chicken muscle and 52 egg samples that were commercially available in Tokyo, Japan. The hydrocortisone concentration was 0.9–41.2 µg kg?1 in all bovine muscle samples, with an average of 7.7 µg kg?1 and a median of 6.2 µg kg?1. The progesterone concentration in 50 samples exceeded the limit of quantification (LOQ) and reached a maximum of 95.4 µg kg?1. Hydrocortisone was also detected in all swine muscle samples at concentrations of 2.0–56.0 µg kg?1. Its average and median concentrations amounted to 13.1 and 11.3 µg kg?1, respectively. Twenty-three samples contained progesterone levels surpassing the LOQ, with a maximum concentration of 107.0 µg kg?1. No chicken muscle samples contained any of the analytes. The progesterone concentration was 15.5–200.0 µg kg?1 in all egg samples, with an average of 95.4 µg kg?1 and a median of 90.5 µg kg?1.  相似文献   

11.
During 2012–2014, 170 samples of export quality raisins were collected from different vendors in Pakistan. The collected samples were analysed for the presence of aflatoxins (AFs) and Ochratoxin A (OTA) contamination using high-performance liquid chromatography technique. The limit of detection and limit of quantification of AFs/OTA were 0.12/0.10 and 0.36/0.30 µg kg?1, respectively. Only 5% of the samples were contaminated with AFs, ranging 0.15–2.58 µg kg?1 with a mean of 0.05 ± 0.26 µg kg?1. None of the raisin samples exhibited AFs contamination above the maximum limit (ML = 4 µg kg?1) as set by the European Union (EU). About 72% of the samples were contaminated with OTA, ranging 0.14–12.75 µg kg?1 with a mean of 2.10 ± 1.9 µg kg?1. However, in 95.3% of the tested samples, OTA level was lower than the ML of 10 µg kg?1 as regulated by the EU. Apparently, a strict and continuous monitoring plan, including regulatory limits, improves food safety and quality for all types of commodities.  相似文献   

12.
The aim of this study was to assess mycotoxin contamination of crops grown by rural subsistence farmers over two seasons (2011 and 2012) in two districts, Vhembe District Municipality (VDM, Limpopo Province) and Gert Sibande District Municiality (GSDM, Mpumalanga Province), in northern South Africa and to evaluate its impact on farmers’ productivity and human and animal health. A total of 114 maize samples were collected from 39 households over the two seasons and were analysed using a validated liquid chromatography-tandem mass spectrometry mycotoxins method. Aflatoxin B1 (AFB1) occurrence ranged from 1 to 133 µg kg?1 in VDM while AFB1 levels in GSDM were less than 1.0 µg kg?1 in all maize samples. Fumonisin B1 levels ranged from 12 to 8514 µg kg?1 (VDM) and 11–18924 µg kg?1 (GSDM) in 92% and 47% positive samples, respectively, over both seasons. Natural occurrence and contamination with both fumonisins and aflatoxins in stored home-grown maize from VDM was significantly (p < 0.0001) higher than from GSDM over both seasons.  相似文献   

13.
The first objective of this study was the validation of an efficient multi-analyte method for the simultaneous detection and quantification of mycotoxins in maize silage, by reverse-phase liquid chromatography coupled with electrospray ionisation triple quadrupole mass spectrometry (LC-HESI-MS/MS). A simple liquid/solid extraction was performed either with clean-up on Mycospin 400 columns or without any clean-up. Almost all the target mycotoxins showed highly-suppressed signals in the presence of a matrix, emphasising the need to quantitate mycotoxins by means of matrix-matched calibrations. An alternative validation method based on ISO 11843 and on a single factor balanced design was implemented. The achieved average recoveries from spiked samples at three levels ranged from 60% to 122% with relative standard deviations (rsd) below 11%. Limits of Detection (LODs) and Limits of Quantification (LOQs) were between 0.02–17.1 µg kg?1 and 0.06–57 µg kg?1. The calculated repeatability and within-lab reproducibility ranged from 5.2 to 23.2% and from 7.2 to 23.9%, respectively. Finally, the decision limit and detection capacity, CCα and CCβ, were calculated for all mycotoxins having regulated/recommended contents in feed. The validated method was applied to 148 samples collected over two years in 19 dairy farms from Galicia (NW Spain). Of the analysed samples, 62% contained at least one mycotoxin. Zearalenone (ZEA), deoxynivalenol (DON), fumonisins B1 and B2, roquefortine C, α-zearalenol, β-zearalenol, enniatins B and B1, andrastin A, marcfortine A, verruculogen and mycophenolic acid were quantified, the highest average detection frequency being for enniatin B (51%). DON, mycophenolic acid and ZEA plus metabolites (α-zearalenol, β-zearalenol) were the most abundant mycotoxins.  相似文献   

14.
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   

15.
ABSTRACT

The detection of mycotoxin contamination in foodstuffs is highly significant for public health. Herein we report an analytical method based on magnetic solid-phase extraction (MSPE) and UPLC-MS/MS for the simultaneous determination of mycotoxins, including fumonisins B1 (FB1), zearalenone (ZON) and ochratoxin A (OTA), in vegetable oil. Magnetic nanoparticles coated with double layers of silicon dioxide were synthesised and found to be an effective MSPE adsorbent for mycotoxins. The proposed MSPE procedure serves not only for sample clean-up but also for mycotoxin enrichment that enhances greatly the assay’s sensitivity. Under the selected MSPE conditions, linear matrix-matched calibration curves were obtained for mycotoxins in a concentration range from 0.178 to 625 μg kg–1. The limits of detection were 0.210 μg kg–1 for FB1, 0.0800 μg kg–1 for OTA and 1.03 μg kg–1 for ZON. The proposed MSPE UPLC-MS/MS method was applied for the determination of mycotoxins in vegetable oil samples, including maize oil, rapeseed oil and soybean oil. ZON was detected in a maize oil at 101 μg kg–1, which is below the European Union limit of 200 μg kg–1 in foodstuffs.  相似文献   

16.
The presence of ochratoxin A (OTA), fumonisin B2 (FB2) and black aspergilli in raisins from Western Greece regions (Messinia, Corinthia, Achaia, Ilia and Zante Island) was investigated in relation to the different geographic and climatic conditions in the 2011 growing season. The biseriate species Aspergillus niger “aggregate” and A. carbonarius were mainly identified. The population of A. niger “aggregate” species occurred in all raisin samples at colony-forming units (CFU) concentrations significantly higher (mean 2.2 × 105 CFU g?1 homogenate) than those of A. carbonarius population (mean 4.9 × 103 CFU g?1 homogenate), which occurred in 80% of the raisin samples. OTA was found in 73% of the samples at levels ranging from 0.1 µg kg?1 to 98.2 µg kg?1, with the highest level occurring in a raisin sample from Ilia that also contained the highest level of A. carbonarius. The European Union legal limit for OTA was exceeded in 15% of the raisin samples. FB2 was found in 29% of the raisin samples at levels ranging from 7.1 µg kg?1 to 25.5 µg kg?1, with 20% of the samples co-occurring with OTA. Principal-component analysis was applied to levels of mycotoxins, fungal contamination, geographical data and environmental conditions recorded in the harvesting (August) or drying (September) period. Principal-component analysis clearly indicated a good direct correlation of rainfall and relative humidity with OTA and A. carbonarius contamination. A lack of clustering was observed when A. niger and FB2 contamination were considered. This is the first report on the co-occurrence of the mycotoxins OTA and FB2 in dried vine fruits from Greece.  相似文献   

17.
In antibiotic residue analyses the first step of screening is just as important as the following steps. Screening methods need to be quick and inexpensive, but above all sensitive enough to detect the antibiotic residue at or below the maximum residue limit (MRL). In the case of a positive result, the next step is conducted and further methods are used for confirmation. MRLs stated in European Union Regulation 37/2010 for tetracyclines in raw milk are: 100 µg kg–1 for tetracycline, 100 µg kg–1 for oxytetracycline, 100 µg kg–1 for chlortetracycline and no limit for doxycycline because it is prohibited for use in animals from which milk is produced for human consumption. The current five-plate microbiological screening method for the detection of antibiotic residues in raw milk was found to be simple and inexpensive, but not specific, sensitive and reliable enough to detect tetracycline at MRL in routine raw milk screening procedures. Spiking samples with tetracycline at the MRL level and applying them on Bacillus cereus ATCC 11778 microbiological plates often gave false-negative results, indicating that tetracyclines may have to be inactivated or masked. Tetracyclines seem to bind to a certain component in milk. Consequently, when applying samples to the B. cereus microbiological plate the antibiotic cannot inhibit the growth of B. cereus which disables the formation of inhibition zones on the test plate. After adding the appropriate amount of citric acid into the milk samples, we solved the problem of false-negative results. During the validation 79 samples of milk were spiked with tetracyclines at different concentrations: 100 µg kg–1 for tetracycline, 100 µg kg–1 for oxytetracycline, 80 µg kg–1 for chlortetracycline and 30 µg kg–1 for doxycycline. Concentrations used in the validation matched the requirements for MRLs (they were either at or below the MRLs) stated in European Union Regulation 37/2010. The sensitivity of the validation was 100%.  相似文献   

18.
The development and validation of a method to determine flonicamid and its metabolites as TFNA (4-trifluoromethylnicotinic acid), TFNG (N-(4-trifluoromethylnicotinoyl) glycine) and TFNA-AM (4-trifluoromethylnicotinamide) in bell pepper samples by ultra-high-performance liquid chromatography coupled to Orbitrap mass spectrometry (UHPLC-Orbitrap-MS) was performed. A fast and simple extraction procedure with acidified acetonitrile and salts (magnesium sulfate and sodium chloride) was used. The methodology was validated, checking for specificity, recovery, precision, limits of detection (LODs) and limits of quantification (LOQs). The recoveries ranged from 84% to 98%, and precisions were lower than 17%. Finally, LODs ranged from 1 µg kg–1 (flonicamid) to 6 µg kg–1 (TFNA-AM), while LOQs ranged from 10 µg kg–1 (flonicamid) to 30 µg kg–1 (TFNA-AM). Bell pepper samples were analysed and concentrations up to 98 µg kg–1 (flonicamid) were detected, although the sum of flonicamid and metabolites did not exceed the maximum residue limit (MRL) set by the European Union.  相似文献   

19.
This survey reports the occurrence of fumonisins (FBs) and fungi in dry soybeans sold for human consumption. The variation levels were 138–1495 µg kg?1 and 178–552 µg kg?1 for FB1 and FB2, respectively. In addition, potentially toxigenic fungi as Fusarium, Aspergillus and Penicillium genera were isolated in the samples. These can be considered as indicator-toxin and can produce considerable amounts of mycotoxins. Despite FB presence in the soybeans for human consumption, there is no legal regulation. Therefore, it is important to emphasise the need for frequent monitoring of these contaminants in soybeans.  相似文献   

20.
Among Fusarium mycotoxins, deoxynivalenol (DON) is the most common contaminant in case of cereals and cereal-based foods in Hungary. In this study, Hungarian wheat (n = 305), maize (n = 108), wheat flour (n = 179) and pasta (n = 226) samples were analysed (N = 818). The samples were collected during 2008–2015 in Hungary. Applied methods of analysis were enzyme-linked immunosorbent assay and liquid-chromatography coupled with a mass spectrometer. Results were compared and evaluated with Hungarian weather data. Among cereal samples, in 2011, wheat was contaminated with DON (overall average ± standard deviation was 2159 ± 2818 µg kg?1), which was above the maximum limit (ML). In case of wheat flour and pasta, no average values above ML were found during 2008–2015, but higher DON contamination could be observed in 2011 as well (wheat flour: 537 ± 573 µg kg?1; pasta: 511 ± 175 µg kg?1).  相似文献   

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