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1.
To determine differences in mean aflatoxin contamination and subsample variance from dry and slurry homogenizations, 10 kg of six different, naturally contaminated dried fig samples were collected from various exporting companies in accordance with the EU Commission Directive. The samples were first dry-mixed for 5 min using a blender and sub-sampled seven times; the remainder was slurry homogenized (1 : 1, v/v) and sub-sampled seven times. Aflatoxin B1 and total aflatoxin levels were recorded and coefficient of variations (CV) computed for all sub-samples. Only a small reduction in sub-sample variations, indicated by the lower CV values, and slight differences in mean aflatoxin B1 and total aflatoxin levels were observed when slurry homogenization was applied. Therefore, 7326 dried figs, destined for export from Turkey to the EU and collected during the 2008 crop year, were dry-homogenized and tested for aflatoxins (B1, B2, G1 and G2) by immunoaffinity column clean-up using RP-HPLC. While 34% of the samples contained detectable levels of total aflatoxins (0.20–208.75 µg kg?1), only 9% of them exceeded the EU limit of 4 µg kg?1 in the range 2.0–208.75 µg kg?1, respectively. A substantial increase in the incidence of aflatoxins was observed in 2008, most likely due to the drought stress experienced in Aydin province as occurred in 2007.  相似文献   

2.
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   

3.
The occurrence of aflatoxins (AF) B1, B2, G1, G2 and cyclopiazonic acid (CPA) in feeds, and AFM1 and CPA in milk was determined in dairy farms located in the northeastern region of São Paulo state, Brazil, between October 2005 and February 2006. AF and CPA determinations were performed by HPLC. AFB1 was found in 42% of feed at levels of 1.0–26.4 µg kg?1 (mean: 7.1 ± 7.2 µg kg?1). The concentrations of AFM1 in raw milk varied between 0.010 and 0.645 µg l?1 (mean: 0.104 ± 0.138 µg l?1). Only one sample was above the tolerance limit adopted in Brazil (0.50 µg l?1) for AFM1 in milk. Regarding CPA in feed, six (12%) samples showed concentrations of 12.5–153.3 µg kg?1 (mean: 57.6 ± 48.7 µg kg?1). CPA was detected in only three milk samples (6%) at levels of 6.4, 8.8 and 9.1 µg l?1. Concentrations of aflatoxins and CPA in feed and milk were relatively low, although the high frequency of both mycotoxins indicates the necessity to continuously monitor dairy farms to prevent contamination of feed ingredients.  相似文献   

4.
In Mexico, maize tortillas are consumed on a daily basis, leading to possible aflatoxin exposure. In a survey of 396 2-kg samples, taken over four sampling days in 2006 and 2007 from tortilla shops and supermarkets in Mexico City, aflatoxin levels were quantified by HPLC. In Mexico, the regulatory limit is 12?µg?kg?1 total aflatoxins for maize tortillas. In this survey, 17% of tortillas contained aflatoxins at levels of 3–385?µg?kg?1 or values below the limit of quantification (<LOQ) and, of these, 13% were >12?µg?kg?1 and 87% were below the regulatory limit. Average aflatoxin concentrations in 56 contaminated samples were: AFB1 (12.1?µg?kg?1); AFB2 (2.7?µg?kg?1); AFG1 (64.1?µg?kg?1) and AFG2 (3.7?µg?kg?1), and total AF (20.3?µg?kg?1).  相似文献   

5.
Chilli peppers from Pakistan are consumed locally and also exported. Their quality is compromised by aflatoxins (AF) contamination. AF in chillies from rural, semi-rural and urban areas of the Punjab region of Pakistan were determined. Twenty-three (52.3%), 22 (50%) and 29 (65.9%) samples from rural, semi-rural and urban areas respectively, contained levels of aflatoxins which exceeded the European Union limits of >5?µg?kg?1 for AFB1 and >10?µg?kg?1 for total AF that apply to spices. Mean values for AFB1 in ground samples were 23.8, 14.8 and 14.0?µg?kg?1 for rural, semi-rural and urban areas, respectively. Mean total AF in ground samples were 27.7, 17.7 and 16.2?µg?kg?1 from equivalent locations. Eleven (50%), 12 (54.5%) and 14 (63.6%) whole samples from rural, semi-rural and urban areas, respectively, contained total levels of AF that exceeded European Union limits. The data indicate that individual localities have particular problems. In conclusion, the concentrations were often greater than the statutory limits set by the European Union.  相似文献   

6.
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   

7.
A total of 126 local and imported samples of commercial white and black pepper in Malaysia were analysed for aflatoxins B1, B2, G1 and G2 (AFB1, AFB2, AFG1, AFG2) content using high-performance liquid chromatography (HPLC) with a fluorescence detector (FD). An acetonitrile–methanol–water (17 : 29 : 54; v/v) mixture was used as a mobile phase and clean-up was using an immunoaffinity column (IAC). Seventy out of 126 (55.5%) samples were contaminated with total aflatoxins, although only low levels of aflatoxins were found ranging from 0.1 to 4.9 ng g?1. Aflatoxin B1 showed the highest incidence of contamination and was found in all contaminated samples. There was a significant difference between type of samples and different brands (p < 0.05). The results showed black peppers were more contaminated than white peppers.  相似文献   

8.
A survey was conducted to determine the occurrence of fumonisin B1, B2 and B3 during 2007 in 186 samples of organic and conventional locally available corn products. Samples included baby food (n = 62), corn flour (11), cornflakes (23), pasta (14), cookies (17) and other corn products (59) were obtained from popular markets of Valencia (Spain) and Perugia (Italy). The analytical method used pressurized liquid extraction and liquid chromatography/electrospray ionization tandem mass spectrometry with a triple quadrupole (QqQ) analyser. Of the 104 Spanish samples, 22% contained levels in the range of 2–449 µg kg?1, 2–229 µg kg?1 and 6–105 µg kg?1 for FB1, FB2 and FB3, respectively, while 19 (23%) of the 82 Italian samples were positive with quantifiable levels between 2–235 µg kg?1, 3–187 µg kg?1, and 4–40 µg kg?1 for fumonisins B1, B2 and B3, respectively. Overall, none of the Italian samples and only one organic baby food sample from a Spanish market was above the maximum permitted levels established by European legislation. Fumonisins were found mostly in corn flour followed by cookies and cornflakes. Eleven samples from Spain and nine samples from Italy were organic products, being contaminated the 72% and 77% of the samples, respectively. Analysis of the results showed that levels of fumonisins in corn products were similar in Italy and Spain. The safety of fumonisin intake through corn products was demonstrated by the calculation of the estimated daily intake of both populations considering organic and conventional products separately, which ranged from 1.7 × 10?3 to 0.72 µg kg?1 bw day?1 and comparing them with the provisional maximum total daily intake (PMTDI) of 2 µg kg?1 bw day?1 established by the European Union.  相似文献   

9.
Surveys were carried out between 2007 and 2009 to determine the aflatoxin B1 content of 3345 commercial Turkish foodstuffs supplied by producers for testing for their own purposes or for export certification. To simplify the reporting of data, foods were categorized as: 1, high sugar products with nuts; 2, nuts and seeds; 3, spices; 4, grain; 5, cocoa products; 6, dried fruit and vegetables; 7, processed cereal products; 8, tea; and 9, baby food and infant formula. Aflatoxin analysis was carried out by high-performance liquid chromatography with fluorescence detection after immunoaffinity column clean-up, with a recoveries ranging from 91% to 99%, depending on the matrix. Of the 3345 samples analysed, 94% contained aflatoxin B1 below the European Union limit of 2 µg kg?1, which applies to nuts, dried fruit, and cereals products. The 6% of the 206 contaminated samples were mainly nuts and spices. For pistachios, 24%, 38%, and 42% of the totals of 207, 182, and 24 samples tested for 2007, 2008 and 2009, respectively, were above 2 µg kg?1, with 50 samples containing aflatoxin B1 at levels ranging from 10 to 477 µg kg?1.  相似文献   

10.
A sensitive and selective analytical method for the simultaneous separation and quantitative determination of aflatoxins B1, B2, G1 and G2 in foodstuffs and materials for feed has been validated. The method is based on high performance liquid chromatography with on-line post-column photochemical derivatization and fluorescence detection. The chromatographic separation of aflatoxins was accomplished using a C18 column eluted with an isocratic mobile phase consisting of water, methanol and acetonitrile. The sample preparation required a simple extraction of aflatoxins with MeOH/H2O (80:20, v/v) and a purification step by immunoaffinity column cleanup. The total analysis time, including sample preparation and chromatographic separation, did not exceed 40 min with a run time of 10 min. The on-line photochemical derivatization ensures better results in terms of simplicity, sensitivity and reproducibility with respect to chemical derivatization techniques, and provides an increase of the peak resolution and an extent of automation in comparison with the electrochemical ones. The procedure for the determination of aflatoxins in food samples and cereals for animal consumption was extensively validated following Regulation (EC) No. 882/2004. Detection limits in wheat bran samples of 0.08 µg kg?1 for AFB1, 0.02 µg kg?1 for AFB2, 0.16 µg kg?1 for AFG1 and 0.04 µg kg?1 for AFG2 were attained. The method allows high recovery with mean values ranging from 72 to 94% and it satisfies the necessary requirements for sensitivity, linearity, selectivity, precision and ruggedness, demonstrating the conformity of the method with provisions of Regulation (EC) No. 401/2006.  相似文献   

11.
This survey was carried out to evaluate the occurrence of total aflatoxins (AFs; B1+B2+G1+G2) in unpacked composite spices. A total of 75 samples of composite spices such as biryani, karhai, tikka, nihari and korma masalas were collected from local markets of Karachi, Pakistan, and analysed using HPLC technique. The results indicated that AFs were detected in 77% (n = 58) samples ranging from 0.68 to 25.74 µg kg?1 with a mean of 4.63 ± 0.95 µg kg?1. In 88% (n = 66) samples, AFs level was below the maximum limits (ML = 10 µg kg?1) as imposed by EU. Furthermore, 61% (n = 46) tested samples contained AFs level between 1 and 10 µg kg?1, 9% (n = 7) exhibited AFs contamination ranged 10?20 µg kg?1 and only 3% (n = 2) of the investigated samples contained AFs levels higher than the ML of 20 µg kg?1 for total aflatoxins as set by the USA. It was concluded that there is need to establish a strict and continuous national monitoring plan to improve safety and quality of spices in Pakistan.  相似文献   

12.
A total of 85 walnut samples collected between October 2012 and April 2013 in different provinces of Turkey were analysed for the presence of aflatoxins (AFs). The method involved methanol–water extraction, clean-up with immunoaffinity columns and a sensitive high-performance liquid chromatography coupled with fluorescence detection after post-column derivatisation. The method was validated for selectivity, linearity, trueness, precision, limit of detection and limit of quantification (LOQ), which met the performance criteria as set by EC regulation No. 401/2006. LOQs were 0.07, 0.04, 0.09 and 0.05 µg kg–1 for AFB1, AFB2, AFG1 and AFG2, respectively. AFs were present in 9.4% of walnut samples (8/85) at total AFs levels ranging from 0.09 to 15.4 µg kg–1. Only one of eight walnut samples exceeded the European Union limit of 2 and 4 µg kg–1 for AFB1 and total AFs, respectively.  相似文献   

13.
Mycotoxin analysis is usually carried out by high performance liquid chromatography after immunoaffinity column cleanup or in enzyme-linked immunosorbent assay tests. These methods normally involve determination of single compounds only. EU legislation already exists for the aflatoxins, ochratoxin A and patulin in food, and legislation will come into force for deoxynivalenol, zearalenone and the fumonisins in 2007. To enforce the various legal limits, it would be preferable to determine all mycotoxins by routine analysis in different types of matrices in one single extract. This would also be advantageous for HACCP control purposes. For this reason, a multi-method was developed with which 33 mycotoxins in various products could be analysed simultaneously. The mycotoxins were extracted with an acetonitrile/water mixture, diluted with water and then directly injected into a LC–MS/MS system. The mycotoxins were separated by reversed-phase HPLC and detected using an electrospray ionisation interface (ESI) and tandem MS, using MRM in the positive ion mode, to increase specificity for quality control. The following mycotoxins could be analysed in a single 30-min run: Aflatoxins B1, B2, G1 and G2, ochratoxin A, deoxynivalenol, zearalenone, T-2 toxin, HT-2 toxin, α-zearalenol, α-zearalanol, β-zearalanol, sterigmatocystin, cyclopiazonic acid, penicillic acid, fumonisins B1, B2 and B3, diacetoxyscirpenol, 3- and 15-acetyl-deoxynivalenol, zearalanone, ergotamin, ergocornin, ergocristin, α-ergocryptin, citrinin, roquefortin C, fusarenone X, nivalenol, mycophenolic acid, alternariol and alternariol monomethyl ether. The limit of quantification for the aflatoxins and ochratoxin A was 1.0 µg kg?1 and for deoxynivalenol 50 µg kg?1. The quantification limits for the other mycotoxins were in the range 10–200 µg kg?1. The matrix effect and validation data are presented for between 13 and 24 mycotoxins in peanuts, pistachios, wheat, maize, cornflakes, raisins and figs. The method has been compared with the official EU method for the determination of aflatoxins in food and relevant FAPAS rounds. The multi-mycotoxin method has been proven by the detection of more than one mycotoxin in maize, buckwheat, figs and nuts. The LC–MS/MS technique has also been applied to baby food, which is subject to lower limits for aflatoxin B1 and ochratoxin A, ergot alkaloids in naturally contaminated rye and freeze-dried silage samples.  相似文献   

14.
To estimate daily intake of aflatoxins from peanut products consumed by the population of Paraná State (Brazil), 100 samples of peanut products were collected between July 2006 and April 2007. Aflatoxins were determined by an HPLC method with fluorescence detection. There was a 50% occurrence of aflatoxins (B1, B2, G1 and G2) in concentrations ranging from 0.5 to 113?ng?g?1, with 13 samples with levels above 20?ng?g?1. Intake was calculated for average and high adult consumers of peanut products and it was compared with provisional maximum tolerable daily intake (PMTDI). The estimated probable daily intake (PDI) for aflatoxin B1 (AFB1) varied from 0.6 to 10.4?ng?kg?1?bw?day?1, exceeding the PMTDI of 0.4?ng?kg?1?bw?day?1 for carriers of hepatitis B virus.  相似文献   

15.
The occurrence of aflatoxin (aflatoxin B1, aflatoxin B2, aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2)) and heavy metal (Pb, Cd, As and Hg) contamination was determined in 40 industrially produced animal feed samples which were collected from the southwest of Iran. The results indicated that 75% of samples were contaminated by four aflatoxins and the level of AFB1 and sum of aflatoxins were higher than the permissible maximum levels in Iran (5 and 20 µg kg?1, respectively) in all feed samples. A positive correlation was found between four types of aflatoxins in all the tested samples (p < 0.01) and the positive correlation between AFG1 and AFG2 was significant (r2 = 0.708). All feed samples had lead concentrations lower than the maximum EU limit, while 5%, 17% and 42.5% of feed samples had As, Cd and Hg concentrations higher than the maximum limits, respectively.  相似文献   

16.
A survey of moulds and mycotoxins was performed on 99 rice samples taken from the Swedish retail market. The main objective was to study the mould and mycotoxin content in basmati rice and rice with a high content of fibre. Samples of jasmine rice as well as long-grain rice were also included. The samples were analysed for their content of ochratoxin A (high-performance liquid chromatography (HPLC)), aflatoxin B1, B2, G1, and G2 (HPLC, RIDA®QUICK), and mould (traditional cultivation methods in combination with morphological analysis). The majority of samples were sampled according to European Commission Regulation 401/2006. Subsamples were pooled and mixed before milling and both mould and mycotoxin analyses were performed on milled rice. The results showed that the majority of basmati rice (71%) and many jasmine rice samples (20%) contained detectable levels of aflatoxin B1 (level of quantification = 0.1 µg aflatoxin kg?1 rice). Two samples of jasmine rice and ten basmati rice samples contained levels over the regulated European maximum limits of 2 µg kg?1 for aflatoxin B1 or 4 µg kg?1 for total aflatoxins. Aspergillus was the most common mould genus isolated, but also Penicillium, Eurotium, Wallemia, Cladosporium, Epicoccum, Alternaria, and Trichotecium were found. The presence of Aspergillus flavus in 21% of the samples indicates that incorrect management of rice during production and storage implies a risk of mould growth and subsequent production of aflatoxin. Rough estimates showed that high rice consumers may have an intake of 2–3 ng aflatoxin kg?1 bodyweight and day?1 from rice alone. This survey shows that aflatoxin is a common contaminant in rice imported to Europe.  相似文献   

17.
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   

18.
A sensitive and reliable multi-mycotoxin method was developed for the simultaneous determination of 16 toxicological important mycotoxins, such as aflatoxins B1, B2, G1, and G2; enniatins A, A1, B, and B1; beauvericin; ochratoxin A; fumonisin B1, B2, and B3; diacetoxyscirprenol; HT-2; and T-2 toxin in dried fruits using liquid chromatography combined with electrospray ionization-triple quadrupole tandem-mass spectrometry. Mycotoxins have been extracted from the samples using a modified quick, easy, cheap, effective, rugged, and safe procedure. The method was based on a single extraction with acidified acetonitrile, followed by partitioning with salts, avoiding any further clean-up step. Limits of detections ranged from 0.08 to 15 μg kg?1 and limits of quantification ranged from 0.2 to 45 μg kg?1, which were below the legal limit set by the European Union for the legislated mycotoxines. The recoveries in spiked samples ranged from 60 to 135 % except for beauvericin using matrix-matched calibration curves for quantification, with good inter- and intraday repeatability (respective relative standard deviation ≤20 and 9 %). The developed method was applied to 15 commercial dried fruits: raisins, figs, apricots, plums, and dates purchased in local markets from Spain. Among the mycotoxins studied, enniantins and aflatoxins were the most predominant mycotoxins.  相似文献   

19.

ABSTRACT

The main focus of our study was to implement a rapid, inexpensive and reliable method that could be utilized to check the cereals for safety (i.e., screening for total aflatoxins, as well as individual B1, B2, G1, G2 aflatoxins and ochratoxin A). We developed a protocol by which we were able to isolate mycotoxins from cereals collected from different regions of Romania. After extraction in chloroform, the mycotoxins were separated by thin‐layer chromatography (TLC) and quantified using densitometry. Forty‐three samples of different cereals (wheat, maize, rye and Triticale) were analyzed. Twenty‐five of the 43 samples (58.14% of the total number) were found to be contaminated with different mycotoxins in various concentrations: aflatoxin B1 (1.6–5.7 µg/kg), aflatoxin B2 (0.89–4 µg/kg), aflatoxin G1 (1.2–5.76 µg/kg), aflatoxin G2 (0.96–3.4 µg/kg) and/or 4.3–30 µg/kg ochratoxin A. The concentration of total aflatoxin contamination ranged from 11.2 to 10.8 µg/kg. Among the different cereals, the highest number of contaminated samples was found to be in the wheat samples (62.5%). The method outlined in this study has been adopted already by our laboratory for current analyses of mycotoxins. The results obtained using this method is in compliance with the strict regulatory guidelines developed both in Romania, as well as in the European Union.

PRACTICAL APPLICATIONS

Thin‐layer chromatography (TLC) is a rapid, inexpensive and convenient method that can be used routinely to screen for mycotoxins. This article describes the detailed procedures for the extraction, purification and quantification of aflatoxins and ochratoxin A, using TLC. Using this method one can identify concomitantly five different mycotoxins and by coupling it with densitometry a quantitative determination is also possible. Therefore, this could become a routine technique in regional laboratories responsible for checking agrifood safety.  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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