[Show abstract][Hide abstract] ABSTRACT: A method for the determination of fumonisin B1 (FB1) and B2 (FB2) in different commercial maize-based products
for infants and young children was developed and tested in a limited validation study involving 3 laboratories. The
method used extraction at 55 °C with an acidic mixture of methanol-acetonitrile-phosphate/citrate buffer, clean-up
through immunoaffinity column and fumonisin determination by high performance liquid chromatography with
automated pre-column derivatisation with o-phthaldialdehyde. Recovery experiments were performed at five spiking
levels in the ranges of 80-800 μg/kg FB1 and 20-200 μg/kg FB2. Mean recoveries ranged from 83 to 97% for FB1 and
from 61 to 78% for FB2. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 5 to
12% for FB1 and from 8 to 13% for FB2, whereas relative standard deviation for between-laboratory reproducibility
(RSDR) ranged from 6 to 10% for FB1 and from 9 to 16% for FB2. The limit of quantification of the method (signal
to noise ratio of 6) was 2.8 μg/kg for FB1 and 2.2 μg/kg for FB2. Fumonisins were found in 6 out of 19 maize-based
baby foods obtained from the Italian retail market at levels up to 53 μg/kg.
Full-text · Article · May 2010 · World Mycotoxin Journal
[Show abstract][Hide abstract] ABSTRACT: Acrylamide, a probable human carcinogen, was detected in various heat-treated foods such as French fries and potato crisps. Recently, positive associations have been found between dietary acrylamide intakes, as estimated with a food frequency questionnaire using an acrylamide database, and cancer risk in some epidemiological studies. As acrylamide levels vary considerably within the same type of foods, a validation study was performed to investigate whether use of an acrylamide food database containing calculated mean acrylamide content, based on extensive sampling and chemical analysis of Dutch foods (several samples per food), can classify subjects with respect to true acrylamide intake.
We used the data from a 24-h duplicate diet study. The acrylamide content of 39 Dutch 24-h duplicate diets collected in 2004 was estimated using the mean acrylamide levels of foods available from the database and the menu list, on which the participants of the duplicate diet study had listed the amounts of individual foods and drinks in household units. Next, the acrylamide content of the total duplicate diets was analytically measured and correlated to the estimated acrylamide contents.
The Spearman's correlation coefficient between chemically determined acrylamide content and the calculated acrylamide content of the duplicate diets was 0.82 (P<0.001).
This study indicates that it is possible to classify subjects with respect to acrylamide intake if mean instead of actual content of each food is applied. The database can therefore be applied in epidemiological studies on acrylamide intake and cancer risk, such as the Netherlands Cohort Study on Diet and Cancer.
Full-text · Article · Mar 2010 · European journal of clinical nutrition
[Show abstract][Hide abstract] ABSTRACT: In 2006, a duplicate diet study of children's food was carried out in the Netherlands. Parents or guardians of 123 children collected duplicates of the 24-hour diets. Levels of aflatoxin M1, aflatoxin B1, ochratoxin A, trichothecenes and fumonisins were determined. Aflatoxin M1 was detectable in 10% of the samples, with all toxin levels below the limit of quantification. Aflatoxin B1 could be detected in 80% of the samples, while in 47% of all samples aflatoxin B1 was quantifiable. Ochratoxin A could be quantified in all samples. Deoxynivalenol was quantified in almost every sample, while T-2 and HT-2 toxins could only be quantified in 3.2% and 6.4% of the samples respectively. 15-acetyldeoxynivalenol was detected in 1.6% of the samples. Fumonisin B1 was detected in 28% of the samples and fumonisin B2 in a quarter of merely those samples where fumonisin B1 was detected. In 20% of the samples fumonisin B1 could be quantified and in a quarter of those samples fumonisin B2 could be quantified too. The analytical results were used to estimate levels of daily intake. Only the mean daily intake levels for aflatoxin B1, ochratoxin A, deoxynivalenol and fumonisins B1 and B2 could reliably be estimated. The values were 0.1, 4.1, 291 and 28 ng/kg bw/day respectively, all are well below the corresponding tolerable daily intakes. For aflatoxin B1 a tolerable intake does not exist, but the intake value for this mycotoxin was very low if compared to the value that would result from the intake of food, if it was contaminated with aflatoxin B1 at the EU regulatory limit, specified for baby food. The mean daily intakes of the mycotoxins determined in children's food in the Netherlands are low and implicate that there is no health risk for children due to exposure from the studied mycotoxins.
No preview · Article · Nov 2009 · World Mycotoxin Journal
[Show abstract][Hide abstract] ABSTRACT: Infants have a more restricted diet and they generally consume more food on a body weight basis than adults. Therefore, the
significance and potential health risk of any contaminant in foods consumed by infants is increased and diligent attention
must be paid to this particular area. The present study aims to determine the occurrence of aflatoxin M1 (AFM1), aflatoxin B1 (AFB1) and ochratoxin A (OTA) in processed cereal-based foods (flours) and infant formulae (milk powder) available in the Portuguese
market, both sold as conventional and organic origin. Mycotoxin determination was carried out using a method previously applied
to duplicate diet samples. This method employed chloroform extraction, liquid–liquid extraction, immunoaffinity column (IAC)
cleanup and HPLC analysis with fluorescence detection after post-column derivatisation. Quantification limits were 0.014,
0.004 and 0.028μg kg−1 for AFM1, AFB1 and OTA, respectively. These toxins could only be quantified in 12 of 27 analysed samples (15 positive results): two samples
with AFM1, two samples with AFM1 and OTA, one sample with AFB1 and OTA and seven samples with OTA. Positive results concerned four for AFM1 (26%), one for AFB1 (7%) and ten for OTA (67%). For these samples, contents ranged between 0.017–0.041μg AFM1 kg−1, 0.034–0.212μg OTA kg−1, and one sample had a value of 0.009μg AFB1 kg−1. Considering the presented results, we could provisionally conclude that the presence of these mycotoxins in baby foods does
not constitute a public health problem. These are the first results concerning the occurrence of mycotoxins in marketed baby
foods in Portugal and this is the first study using the HPLC method, proposed for duplicate diets, in baby food sample analysis.
No preview · Article · Mar 2008 · Food Analytical Methods
[Show abstract][Hide abstract] ABSTRACT: An interlaboratory trial for determination of zearalenone (ZON) in baby food and animal feed was conducted. The study involved 39 participants in 16 European Union member states, as well as Turkey, Uruguay, and China, representing a cross-section of industry, and official food control and research institutes. The method is based on immunoaffinity column cleanup followed by high-performance liquid chromatography using fluorimetry (HPLC-FI). The test portion of the sample is extracted with methanol-water (75 + 25, v/v). The sample extract is filtered, diluted, and passed over an immunoaffinity column. ZON is eluted with methanol. The separation and determination of ZON is performed by reversed-phase HPLC-FI with an excitation wavelength of 274 nm and an emission wavelength of 446 nm. Test portions of the samples were spiked at levels of 20 and 30 μg/kg ZON in baby food and at levels of 100 and 150 μg/kg ZON in animal feed. Mean recoveries from each participant ranged from 78 to 119% with an average value of 92% for baby food and from 51 to 122% with an average value of 74% for animal feed. Based on results for spiked samples (blind duplicates at 2 levels), as well as naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in baby food ranged from 2.8 to 9.0%. For animal feed, this value ranged from 5.7 to 9.5%. The relative standard deviation for reproducibility (RSDR) in baby food ranged from 8.2 to 13.3%, and for animal feed this value ranged from 15.5 to 21.4%. The Horwitz ratio (HorRat) in baby food ranged from 0.3 to 0.4, and for animal feed this value ranged from 0.6 to 0.9. The method showed acceptable within- and between-laboratory precision for each matrix, as required by European legislation.
Full-text · Article · Nov 2007 · Journal of AOAC International
[Show abstract][Hide abstract] ABSTRACT: An interlaboratory study was conducted for the determination of deoxynivalenol in baby food and animal feed by high-performance liquid chromatography with UV detection. The study included 14 participants representing a cross section of industry, official food control, and research facilities. Mean recoveries reported ranged from 89% (at 120 microg/kg) to 85% (at 240 microg/kg) for baby food and from 100% (at 200 microg/kg) to 93% (at 400 microg/kg) for animal feed. On the basis of the results for spiked samples (blind duplicates at 2 levels), as well as those for naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in analyses of baby food ranged from 6.4 to 14.0% and in analyses of animal feed, from 6.1 to 16.5%. The relative standard deviation for reproducibility (RSDR) in analyses of baby food ranged from 9.4 to 19.5% and in analyses of animal feed, from 10.5 to 25.2%. The HorRat values ranged from 0.4 to 1.0 and from 0.7 to 1.3, for baby food and animal feed, respectively. The method showed acceptable performance for within-laboratory and between-laboratory precision for each matrix, as required by European legislation.
No preview · Article · Jul 2006 · Journal of AOAC International
[Show abstract][Hide abstract] ABSTRACT: A method was developed for the determination of aflatoxin B1 in medical herbs (senna pods, botanical name Cassia angustifolia; devil's claw, botanical name Harpagophytum procumbens; and ginger roots, botanical name Zingiber officinale). The method, which was tested in a mini-collaborative study by 4 laboratories, is based on an immunoaffinity cleanup followed by reversed-phase high-performance liquid chromatography separation and fluorescence detection after post-column derivatization. It allows the quantitation of aflatoxin B1 at levels lower than 2 ng/g. A second extractant (acetone-water) was tested and compared to the proposed methanol-water extractant. Several post-column derivatization options (electrochemically generated bromine, photochemical reaction, and chemical bromination) as well as different integration modes (height versus area) were also investigated. No differences were found depending on the choice of derivatization system or the signal integration mode used. The method was tested for 3 different matrixes: senna pods, ginger root, and devil's claw. Performance characteristics were established from the results of the study and resulted in HorRat values ranging from 0.12 to 0.75 with mean recoveries from 78 to 91% for the extraction with methanol-water and HorRat values ranging from 0.10-1.03 with mean recoveries from 98 to 103% for the extraction with acetone-water. As a result, the method, with all tested variations, was found to be fit-for-purpose for the determination of aflatoxin B1 in medical herbs at levels of 1 microg/kg and above.
Full-text · Article · May 2006 · Journal of AOAC International
[Show abstract][Hide abstract] ABSTRACT: In the spring and autumn of 1994, a total diet study, in which 123 participants collected duplicates of their 24-hour diets, was carried out. The goal of this study was to determine the mass fractions of a number of analytes in these duplicate diets, so as to be able to establish oral daily intake values. After measurements were carried out for pesticides, PCBs, elements, sterols, nitrate and nitrite, and fatty acids, the duplicate diet study was concluded with analyses for aflatoxin M1, aflatoxin B1 and ochratoxin A. For this purpose a method of analysis was developed, that could simultaneously determine these mycotoxins at very low levels. The method involved chloroform extraction, liquid-liquid extraction, immunoaffinity cleanup and liquid chromatography. The method was supplemented with a procedure to confirm the identity of chromatographic peaks, assumed to represent aflatoxin M1, aflatoxin B1 and ochratoxin A. The method was in-house validated. Recoveries ranged from 68-74% for aflatoxin M1 (at spiking levels from 30-120 ng/kg, c.v. 7.6%), from 95-97% for aflatoxin B1 (at spiking levels from 50-200 ng/kg, c.v. 2.8%), and from 75-84% for ochratoxin A (at spiking levels from 150-600 ng/kg, c.v. 4.3%). Limits of quantitation (defined as signal/noise = 10) were estimated to be 24, 5 and 16 ng/kg lyophilised material for aflatoxin M1, aflatoxin B1 and ochratoxin A respectively. The newly developed method was used to analyse 123 samples of 24-hour diets. Aflatoxin M1 was detectable in 48% of the samples; the toxin contents remained below the limit of quantitation in all samples. Aflatoxin B1 could be detected in 42% of the samples; in 25% of the samples the levels were above the limit of quantitation. Ochratoxin A could be quantified in all samples. The analytical results were further processed to estimate levels of intake. Intake levels for the aflatoxins were very low, and could not reliably be established. The mean ochratoxin A intake was estimated to be 1.2 ng/kg body weight per day. This is well below the tolerable daily intake established by JECFA at 14 ng/kg body weight per day. The current dietary intake of ochratoxin A in the Netherlands is concluded to pose no appreciable health risk.
No preview · Article · Mar 2005 · Food Additives and Contaminants
[Show abstract][Hide abstract] ABSTRACT: Seventy-eight maize-containing foods obtained from retail stores in The Netherlands were analysed for fumonisin B1 contamination. Thirty-six per cent of the samples were contaminated with fumonisin B1 in the range of 8 micrograms kg-1 (limit of detection) to 1430 micrograms/kg-1. Forty-six per cent of the minimally treated maize samples (n = 39; maize for bread production, maize for popcorn, maize flour and polenta) were contaminated with fumonisin B1 in the range of 8-380 micrograms kg-1. Twenty-six per cent of the maize-containing processed foods (n = 39; tostada, canned maize, maize starch, maize bread, popped maize, flour mixes, maize chips and cornflakes) were contaminated with fumonisin B1 in the range of 8-1430 micrograms/kg-1. This survey shows that maize-containing foods in The Netherlands frequently can be contaminated with fumonisin B1.
No preview · Article · May 1998 · Food Additives and Contaminants
[Show abstract][Hide abstract] ABSTRACT: Sixty-two samples of maize imported in The Netherlands and intended for human consumption were screened for the presence and concentration of fumonisin B1. Sixty-one of those samples contained fumonisin B1 with concentrations ranging from 30 to 3350 micrograms kg-1, 11 maize samples contained > 1000 micrograms kg-1. The average fumonisin B1 concentration was 640 micrograms kg-1 for the positive samples and 620 micrograms kg-1 for all samples. Medians were 600 micrograms kg-1 and 550 micrograms kg-1 for positive and all samples, respectively. The results obtained were comparable to results from other studies in maize from various countries.
No preview · Article · May 1998 · Food Additives and Contaminants
[Show abstract][Hide abstract] ABSTRACT: The development of three peanut meal and two compound feed reference materials and the certification of their aflatoxin B1 content is described. The materials were prepared and certified within the Measurements and Testing Programme of the Commission of the European Communities as part of a broad activity to improve accuracy and agreement of results of measurements on food and agriculture. RM 262 (peanut meal) was prepared from uncontaminated peanut products. RM 263 and RM 264 (peanut meals) were prepared from naturally contaminated peanuts which were blended with uncontaminated ones, to achieve the desired aflatoxin B1 mass fractions. RM 375 and RM 376 (compound feeds) were made by blending decontaminated dairy feed together with commercial feed ration and contaminated dairy feed with several feed compounds, respectively. Details are given of the preparation and the investigations to verify homogeneity and stability of the materials. The certification exercise was carried out by 17 laboratories using a variety of extraction and clean-up procedures. Most laboratories used liquid chromatography as the determinative step, although operating under a variety of chromatographic conditions. A few laboratories applied thin layer chromatography with densitometric quantification. Peanut meal RM 262 was certified as containing aflatoxin B1 at a mass fraction of < 3 micrograms/kg, RM 263 at 43.3 +/- 2.1 micrograms/kg and RM 264 at 204 +/- 10 micrograms/kg. Compound feed RM 375 was certified as containing aflatoxin B1 at a mass fraction of < 1 micrograms/kg and RM 376 at 9.2 +/- 0.5 micrograms/kg. The materials can be employed either to establish or confirm a calibration curve, or to check the performance of a method.
No preview · Article · Jul 1994 · Food Additives and Contaminants
[Show abstract][Hide abstract] ABSTRACT: A thin-layer chromatographic method is described for the analysis of aflatoxins in animal liver. Liver samples are extracted with chloroform and phosphoric acid. After filtration, an aliquot is evaporated and defatted by liquid-liquid partitioning. The extract is submitted to silica gel minicolumn cleanup and the final extract is concentrated and submitted to two-dimensional thin-layer chromatography (TLC). The identity of aflatoxins B1 and M1 is confirmed with trifluoroacetic acid (TFA) carried out on the thin-layer plate used for quantitation of these aflatoxins. The method permits the detection and confirmation of aflatoxins in liver in concentrations as low as 0.05 micrograms/kg. Average recoveries for aflatoxin M1 and aflatoxin B1 at spiking levels of 0.2 micrograms/kg were found to be 65% and 85%, respectively. With this method, 73 samples of bovine liver, 70 samples of porcine liver, and 56 samples of chicken liver taken from different slaughterhouses were investigated. In one sample of bovine liver, aflatoxins B1, B2, and M1 could be detected in concentrations of 0.10, 0.03, and 0.08 micrograms/kg, respectively.
No preview · Article · Jan 1990 · Journal of Environmental Pathology Toxicology and Oncology
[Show abstract][Hide abstract] ABSTRACT: A liquid chromatographic (LC) method was developed for the determination of aflatoxins in feedstuffs containing citrus pulp. The feed-stuff sample is extracted with chloroform, followed by Sep-Pak Florisil cartridge cleanup and Sep-Pak C18 cartridge cleanup. The final eluate (water-acetone, 85 + 15, v/v) is submitted to reverse-phase liquid chromatography with water-methanol-acetonitrile (130 + 70 + 40, v/v/v) as mobile phase and postcolumn derivatization with iodine. Citrus components are removed from the extract efficiently. The limit of detection for aflatoxin B1 is less than 1 microgram/kg. Other aflatoxins can also be detected and measured. Recoveries of aflatoxins B1, B2, G1, and G2 for dairy rations spiked at 13, 5, 10, and 4 micrograms/kg were 87, 86, 81, and 82%, respectively. Corresponding coefficients of variation were 3.1, 3.6, 5.2, and 3.8%, respectively.
No preview · Article · Sep 1988 · Journal - Association of Official Analytical Chemists
[Show abstract][Hide abstract] ABSTRACT: Six published methods of analysis for the determination of aflatoxin B1 have been compared for their suitability to determine aflatoxin B1 in feeding stuffs containing citrus pulp. These methods are the official European Community (EC) procedure, four procedures proposed in the European Community to replace this method and a new procedure developed by the authors of this article. In all procedures chloroform is used for initial extraction. Various clean-up systems are then applied. For the ultimate separation and detection, use is made of high performance liquid chromatography (HPLC) in three procedures and two-dimensional thin layer chromatography (TLC) in two procedures. One method allows either HPLC or TLC. All experiments were carried out with samples of a batch of feeding stuff containing citrus pulp, artificially contaminated with aflatoxins B1, B2, G1 and G2 at levels of ca 13, 5, 10 and 4 micrograms/kg respectively. Three methods were found to be suitable: a procedure in which gel permeation clean-up and two-dimensional TLC are used; a procedure in which TLC clean-up and reverse phase HPLC with postcolumn derivatization are used: a procedure in which cartridge clean-up and either HPLC or TLC are used. The latter method is preferred because its efficient clean-up yields a very clean extract, allowing the application of various systems of HPLC or TLC. Published recovery data of these three methods for aflatoxin B1 vary from 85-90% at a level of ca 10 micrograms/kg feeding stuff.
No preview · Article · Jul 1988 · Food Additives and Contaminants