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1.
UK rye-based cereal products were analysed for six major ergot alkaloids using an in-house-validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that distinguished -ine and -inine epimers (isomers). Ergot alkaloids were detected in 25 of 28 samples subject to quantification limits of 1–3 µg kg?1, including all of eleven rye crispbreads that had up to 340 µg kg?1. Continental-style rye breads contained up to 121 µg kg?1. Loaf breads, bread-mix flours, and crackers contained only low levels of alkaloids. Ergotamine, ergocristine, and ergosine were the predominant ergot alkaloids in terms of level and frequency of occurrence. There were no apparent differences in the ergot levels between the organic and non-organic products, although the numbers tested were low. Most rye breads had a ratio of -ines to -inines of about 1.5, and rye crispbreads had lower and more variable -ine to -inine ratios.  相似文献   

2.
Ergot alkaloids are mycotoxins that are undesirable contaminants of cereal products, particularly rye. A method was developed employing clean-up by cation-exchange solid-phase extraction, separation by high-performance liquid chromatography under alkaline conditions and fluorescence detection. It is capable of separating and quantifying both C8-isomers of ergocornine, alpha-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61% +/- 10% with limits of detection from 0.2 to 1.1 microg kg(-1). Twenty-four unknown rye flour samples from Danish mills contained on average 46 microg kg(-1) with a maximum content of 234 microg kg(-1). The most common ergot alkaloids were ergotamine and alpha-ergocryptine including their C8-isomers. A total of 54% of the ergot alkaloids were detected as C(8)-S isomers.  相似文献   

3.
Ergot alkaloids are mycotoxins that are undesirable contaminants of cereal products, particularly rye. A method was developed employing clean-up by cation-exchange solid-phase extraction, separation by high-performance liquid chromatography under alkaline conditions and fluorescence detection. It is capable of separating and quantifying both C8-isomers of ergocornine, alpha-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61% +/- 10% with limits of detection from 0.2 to 1.1 microg kg(-1). Twenty-four unknown rye flour samples from Danish mills contained on average 46 microg kg(-1) with a maximum content of 234 microg kg(-1). The most common ergot alkaloids were ergotamine and alpha-ergocryptine including their C8-isomers. A total of 54% of the ergot alkaloids were detected as C(8)-S isomers.  相似文献   

4.
A sensitive LC–MS/MS method for the simultaneous determination of type A, B and D trichothecenes in cereals is presented. The limits of detection ranged between 0.1 and 0.7 µg kg?1 for all analytes. The method was applied to 289 representatively drawn samples of wheat, rye and oat products. Ninety-four percent of the wheat samples (n = 130), 95% of the rye samples (n = 61) and 100% of the oat samples (n = 98) were contaminated with the type A trichothecenes T-2 and HT-2 toxin. Median levels of T-2/HT-2 (sum of the toxins) were 0.91, 0.53 and 8.2 µg kg?1, respectively. Highest levels were found in wheat bran (24 µg kg?1), rye kernels (3.1 µg kg?1) and oat flakes (85 µg kg?1). All wheat and rye samples and 75% of the oat samples were contaminated with the type B trichothecene deoxynivalenol. Median levels of this toxin were 23, 15 and 0.53 µg kg?1, respectively. Highest levels were found in wheat bran (1160 µg kg?1), rye kernels (288 µg kg?1) and oat flakes (55 µg kg?1). The type B trichothecene nivalenol was detected in 67% of the wheat samples, in 3% of the rye samples and in 24% of the oat samples with highest levels in wheat bran (96 µg kg?1), rye kernels (1.8 µg kg?1) and in oat flakes (17 µg kg?1), respectively. Levels of other type A and B trichothecenes played a minor role, although the rates of contamination were often high. Neither macrocyclic type D trichothecenes (satratoxin G and H, verrucarin A, roridin A) nor diacetylverrucarol and verrucarol (type A trichothecenes), were detected in any of the samples.  相似文献   

5.
An LC-MS/MS multi-method was developed to simultaneously quantify ergot alkaloids (EAs) and tropane alkaloids (TAs) in 113 cereal-based food for infants and young children. To assess yearly variation, samples were collected in 2011, 2012 and 2014. EAs were detected in 54% and TAs in 22% of the samples. Mean EA levels in the three sampling years were 10.6, 6.2 and 8.6 µg kg?1, respectively (maximum: 115.4 µg kg?1), indicating that exposure to EAs would not have exceeded the health-based guidance values set by EFSA in 2012. Mean TA levels were 3.9, 2.4 and 0.4 µg kg?1, respectively (maximum: 80.8 µg kg?1). The acute reference dose for TAs, derived by EFSA in 2013, would have been exceeded by young children when consuming some of the products sampled in 2011–2012. TA levels had decreased drastically in 2014, possibly due to measures taken by producers as response to the EFSA Opinion.  相似文献   

6.
7.
Acrylamide in baked and toasted wheat and rye bread was studied in relation to levels of asparagine in flour, dough, bread and toasts. Asparagine was consumed during bread preparation resulting in reduced acrylamide content in the products. In wheat bread, 12% of the asparagine initially present in the flour (0.14 g kg?1) remained after yeast fermentation and baking; for rye bread, 82% of asparagine remained after sourdough fermentation and baking. Asparagine present in untoasted wheat bread had totally reacted after hard toasting. Toasted wheat and rye bread slices contained 11–161 and 27–205 µg kg?1 acrylamide, respectively, compared to untoasted wheat and rye bread with <5 and 7–23 µg kg?1 acrylamide, respectively. The dietary intake of acrylamide from bread (untoasted) of 2 µg day?1 is relatively low; however, acrylamide exposure from bread increases several fold for people eating toasted bread.  相似文献   

8.
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   

9.
The aims of the study were to obtain information about the occurrence of ochratoxin A (OTA) and citrinin (CIT) in cereals harvested in the Czech Republic and to compare two analytical procedures for detecting OTA. A total of 34 cereal samples, including two matrix reference materials (R-Biopharm, Germany), were analysed. The results were compared with the limit for raw cereal grains used as a foodstuff according to Commission Regulation No. 1881/2006, which allows a maximum OTA level of 5 µg kg?1. Compared were two methods based on the high-performance liquid chromatography principle, one using the immunoaffinity columns OchraTest? (VICAM) and the second based on solvent partition (PART), both followed by fluorescence detection. The highest OTA contents were found in two barley samples. According to the method employed, the results for the first sample (malting barley) were VICAM = 31.43 µg kg?1 and PART = 44.74 µg kg?1. For the second sample (feeding barley) they were VICAM = 48.63 µg kg?1 and PART = 34.40 µg kg?1. Two samples of bread wheat had an OTA content approaching the legal limit (VICAM = 4.71 µg kg?1 and PART = 6.03 µg kg?1; VICAM = 4.12 µg kg?1 and PART = 3.95 µg kg?1). CIT was analysed using the PART method only, and its highest content (93.64 µg kg?1) was found for the malting barley sample with high OTA content (44.74 µg kg?1 as analysed using PART).  相似文献   

10.
Potato crisps are one of the food commodities that contribute most to overall dietary human exposure of acrylamide. This investigation has estimated the dietary exposure to acrylamide form potato crisps in the Spanish population. Sampling of potato crisps (n = 36) from 16 different producers were carried out in March 2008. An average level of 740 µg kg?1 (ranging from 81 to 2622 µg kg?1; minimum to maximum) and a median of 592 µg kg?1 were obtained. Acrylamide levels in marketed potato crisps have been significantly reduced (nearly to 50%) compared with a previous sampling performed 4 years earlier. The observed signal value (90th percentile) was 1377 µg kg?1 with 86% of the samples with acrylamide levels lower than 1000 µg kg?1. Dietary exposure to acrylamide from potato crisp consumption in the total Spanish population was estimated to be 0.042 µg kg?1 body weight day?1 by using a deterministic approach based on the National consumption database. In a second study, dietary exposure (based on a 3-day food record) was determined to be 0.053 µg kg?1 body weight day?1 for the adult population (17–60 years) and 0.142 µg kg?1 body weight day?1 for children (7–12 years). The contribution of potato crisps to the estimated dietary acrylamide exposure of the Spanish population is moderate as compared with other European Member States.  相似文献   

11.
Two microbiological kits based on Bacillus stearothermophilus (Eclipse 50® and Premi®Test) have been evaluated and validated according to the European guideline for the validation of screening methods (January 2010) and in relation to the concentrations recommended by the EU-RL in 2007. Both tests are robust, a fast method and easy to implement. Both tests are applicable to a very large variety of honeys from different floral and geographical origins (rosemary, lavender, scrub, heath, alder, forest, lemon, acacia, chestnut, raspberry, mountain and flowers) as well as honey of different colours (from blank honey to brown honey, including yellow and orange honey). A satisfactory false-positive rate of 5% was obtained for the Eclipse 50® test. The observed detection capabilities CCβ of the Eclipse 50® kit were: chlortetracycline (>75?µg?kg?1), oxytetracycline (≤200?µg?kg?1), tetracycline (>100?µg?kg?1), cloxacillin (≤40?µg?kg?1), tylosin (≤200?µg?kg?1), desmycosin (>400?µg?kg?1), sulfadiazine (≤300?µg?kg?1), sulfadimethoxine (≤250?µg?kg?1), sulfamerazine (>300?µg?kg?1), sulfamethazine (>1000?µg?kg?1), sulfamethizole (>75?µg?kg?1), sulfamethoxazole (≤25?µg?kg?1), sulfanilamide (?1000?µg?kg?1), sulfaquinoxaline (>75?µg?kg?1), sulfathiazole (≤250?µg?kg?1) and lincomycin (>1500?µg?kg?1). These levels were all higher than the recommended concentrations where they exist. Due to its lack of sensitivity, it cannot be recommended for reliable routine use. The observed CCβ of the Premi®Test kit were: chlortetracycline (10?µg?kg?1), oxytetracycline (>10?µg?kg?1), tetracycline (≤10?µg?kg?1), cloxacillin (≤5?µg?kg?1), tylosin (≤10?µg?kg?1), desmycosin (≤15?µg?kg?1), sulfadiazine (≤25?µg?kg?1), sulfadimethoxine (≤25?µg?kg?1), sulfamerazine (≤25?µg?kg?1), sulfamethazine (≤25?µg?kg?1), sulfamethizole (≤25?µg?kg?1), sulfamethoxazole (≤10?µg?kg?1), sulfanilamide (≤25?µg?kg?1), sulfaquinoxaline (≤10?µg?kg?1), sulfathiazole (25?µg?kg?1) and lincomycin (≤25?µg?kg?1). The Premi®Test kit could be recommended for reliable use in routine control due to its low detection capabilities (except for aminoglycosides), but the disadvantage is a high false-positive rate of 14%.  相似文献   

12.
The occurrence of deoxynivalenol (DON) was investigated in 514 cereal-based products (corn-based, n = 125; barley-based, n = 96; wheat-based, n = 94; rice-based, n = 199) marketed in Korea during 2007?2008, and estimates of DON intake were determined. Samples were analysed by high-performance liquid chromatography (HPLC) with ultraviolet light (UV) detection after immunoaffinity clean-up. The limits of detection (LOD) and limits of quantification (LOQ) were 2.2 and 5.6 µg kg–1, respectively. Recoveries and repeatability expressed as coefficients of variation (CV) were 82.3–100% and 2.4–15.3% in beer, bread and dried corn. The incidences and mean levels of DON were 56% and 68.9 µg kg?1 for corn-based products, 49% and 24.1 µg kg?1 for wheat-based products, 43% and 7.5 µg kg?1 for barley-based products, and 16% and 3.4 µg kg?1 for rice-based products, respectively. The estimated daily intake of DON from the consumption of rice-based, wheat-based, barley-based and corn-based products were 0.0038 µg kg?1 bw day?1, 0.0032 µg kg?1 bw day?1, 0.0015 µg kg?1 bw day?1 and 0.0002 µg kg?1 bw day?1, respectively. These values represent 0.38%, 0.32%, 0.25% and 0.01% of the provisional maximum tolerable daily intake (PMTDI) of 1 µg kg?1 bw day?1. These results indicate that rice-based products are major contributors to DON exposure in Korea, even though the current exposure level is unlikely to cause adverse health effects.  相似文献   

13.
The purpose of this study was to measure acrylamide (AA) levels and selected parameters of different traditional Turkish coffees. AA, 5-hydroxymethylfurfural (HMF), total reducing sugar, protein, pH, moisture, dry matter (DM) as well as ash, caffeine and soluble solids content (SSC) in DM, L*, a*, b* colour parameters of coffee samples were determined and the correlation between AA level and these parameters were investigated. A total of 36 coffee samples (20 Turkish, 8 Dibek and 8 Terebinth coffee) from the Turkish market were examined. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was validated for the detection and quantitation of AA in coffee samples. The calibration curve was linear (R2 ≥ 0.999) over the range of 30–1000 μg kg?1. The limit of detection (LOD) and limit of quantification (LOQ) were found as 4.6 μg kg?1 and 15.5 μg kg?1, respectively. The amounts of AA in analysed coffee samples were in the range 31.1 ± 0.6 to 323.4 ± 5.4 µg kg?1. The highest mean AA levels were found in Terebinth coffees (240.3 μg kg?1) followed by Turkish coffees (204.3 µg kg?1) and then Dibek coffees (78.6 µg kg?1). No tested Turkish coffee samples had an AA concentration above the indicative value (450 µg kg?1) for roast coffee recommended by the European Commission (EC) in 2011. In addition, a strong positive correlation was found between HMF values and AA amounts of selected coffee types.  相似文献   

14.
Commercial baby food samples available on the Brazilian market (n = 31) were analysed for furan content using a gas chromatography-mass spectrometry method preceded by solid-phase microextraction. A limit of detection of 0.7 µg kg?1, a limit of quantitation of 2.4 µg kg?1, mean recoveries varying from 80% to 107%, and coefficients of variation ranging from 5.6% to 9.4% for repeatability and from 7.4% to 12.4% for within-laboratory reproducibility were obtained during an in-house validation. The levels of furan found in the samples were from not detected to 95.5 µg kg?1. Samples containing vegetables and meat showed higher furan levels as compared with those containing only fruits. An exposure assessment showed furan intakes up to 2.4 µg kg?1 body weight day?1 (99th percentile) for babies fed exclusively with commercial baby foods. Margins of exposure obtained from intakes estimated in this work indicated a potential public health concern.  相似文献   

15.
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   

16.
This paper reports levels of 3-monochloropropan-1,2-diol (3-MCPD) and 1,3-dichloro-2-propanol (1,3-DCP) in a wide range of food items and estimates their dietary exposure for secondary school students in Hong Kong. Dietary exposure to chloropropanols was estimated using local food consumption data obtained from secondary school students in 2000 and the concentrations of 3-MCPD and 1,3-DCP in food samples taken from the local market. The dietary exposure to 3-MCPD for an average secondary school student consumer was estimated to be 0.063–0.150 µg kg?1 body weight (bw) day?1, whilst that for the high consumer was 0.152–0.300 µg kg?1 bw day?1. Both estimates fell below the provisional maximum tolerable daily intake of 2 µg kg?1 bw established by the Joint Expert Committee on Food Additives (JECFA) and amounted to less than 20% of this safety reference value. The dietary exposure to 1,3-DCP for an average secondary school student consumer was estimated to be 0.003–0.019 µg kg?1 bw day?1, whilst that for the high consumer was 0.009–0.040 µg kg?1 bw day?1. The resulting margins of exposures were of low concern for human health. It could be concluded that both the average and high secondary school student consumers were unlikely to experience major toxicological effects of 3-MCPD and 1,3-DCP.  相似文献   

17.
To evaluate the potential public health risk of ethyl carbamate (EC), EC exposure from fermented foods and beverages for Hong Kong population was estimated. In 276 samples analysed, EC was detected (limit of detection (LOD) at 0.4?µg?kg?1) in 202 samples (73%), with higher levels in fermented red bean curd (150–650?µg?kg?1) and yellow wine (140–390?µg?kg?1), while low or non-detected (ND) in preserved vegetables (ND–10?µg?kg?1) and fermented tea (ND–15?µg?kg?1). The estimated dietary exposure from all fermented foods and beverages was 8.27?ng?kg?1?bw?day?1, while exposure excluding alcoholic beverages was 5.42?ng?kg?1?bw?day?1, with calculated margins of exposure (MOEs) at 3.6?×?104 and 5.5?×?104 respectively. The risk of adverse health effects was low for the average population but higher (MOE?of?103) for high consumers of alcoholic beverages especially habitual drinkers of alcoholic types with high EC contents.  相似文献   

18.
A total of 178 milk samples (94 of buffalo and 84 of cow) were randomly taken from Punjab and the North West Frontier Province (NWFP) of Pakistan (n?=?89 in each province) and analysed for the presence of aflatoxin M1 (AFM1) by HPLC-FLD. From Punjab about 46% of buffalo's and 49% of cow's milks were contaminated with AFM1 as compared with 52% and 51% for milk samples from NWFP, respectively. Overall, the mean AFM1 concentration was 0.046?µg?kg?1 with a maximum of 0.350?µg?kg?1. All samples complied with the Codex Alimentarius limit of 0.50?µg?kg?1 for AFM1 in milk, but 16.3% of samples exceeded the European Union maximum level of 0.05?µg?kg?1. Another set of 415 buffalo's and cow's milk samples (213 morning milks and 202 evening milks) were analysed. Statistical analysis revealed significant differences (p?<?0.05) between mean AFM1 concentrations in milk during the morning (0.043?µg?kg?1) and the evening (0.028?µg?kg?1) lactation times.  相似文献   

19.
A deterministic exposure assessment using the Nusser method that adjusts for within-subject variation and for nuisance effects among Finnish children and adults was carried out. The food consumption data covered 2038 adults (25–74 years old) and 1514 children of 1, 3 and 6 years of age, with the data on foods’ acrylamide content obtained from published Finnish studies. We found that acrylamide exposure was highest among the 3-year-old children (median?=?1.01?µg?kg?1?bw?day?1, 97.5th percentile?=?1.95?µg?kg?1?bw?day?1) and lowest among 65–74-year-old women (median?=?0.31?µg?kg?1?bw?day?1, 97.5th percentile?=?0.69?µg?kg?1?bw?day?1). Among adults, the most important source of acrylamide exposure was coffee, followed by casseroles rich in starch, then rye bread. Among children, the most important sources were casseroles rich in starch and then biscuits and, finally, chips and other fried potatoes. Replacing lightly roasted coffee with dark-roasted, swapping sweet wheat buns for biscuits, and decreasing the acrylamide content of starch-based casseroles and rye bread by 50% would result in a 50% decrease in acrylamide exposure in adults. Among children, substituting boiled potatoes for chips and other friend potatoes and replacing biscuits with sweet wheat buns while lowering the acrylamide content of starch-based casseroles by 50% would lead to acrylamide exposure that is only half of the original exposure. In conclusions, dietary modifications could have a large impact in decreasing acrylamide exposure.  相似文献   

20.
After simultaneous distillation–extraction (SDE) of foods packed in polystyrene (n = 77) and polypropylene cups (n = 42) from 61 different suppliers, coupled capillary gas chromatography–mass spectrometric (HRGC–MS) analyses indicated the presence of diastereomers of 2,2,4-trimethyl–1,3-pentanediol monoisobutyrate (TMPD-MIB; Texanol®), a known coalescent of paints and printing inks. The contaminant was found in 55 and 50% of the polystyrene and polypropylene packed samples, respectively. Amounts ranged 1.2–64.5 µg kg?1 in polystyrene cups (average 25.1 µg kg?1) and 0.9–45.7 µg kg?1 in polypropylene cups (average 10.8 µg kg?1). The origin of Texanol® in the printed plastic cups was demonstrated by separate HRGC–MS analysis, showing amounts in the higher µg kg?1 range. In addition, the presence of two pairs of enantiomers, both found to be racemic by enantioselective multi-dimensional gas chromatography–mass spectrometry (enantio-MDGC–MS), excluded it being of natural origin. The detection limit of overall procedure (DLOP) and the reliable quantification limit (RQL) were 0.2 and 0.9 µg kg?1, respectively. As the diester, 2,2,4-trimethyl–1,3-pentanediol diisobutyrate (TXIB), is on the EU list of regulated substances (restricted to single-use gloves only) with a migration limit of 5 mg kg?1 in food and is metabolised rapidly by hydrolysis, the observed migration of the monoester Texanol® at the µg kg?1 level poses no risk of adverse effects.  相似文献   

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