Ergot alkaloids in rye flour determined by solid-phase cation-exchange and high-pressure liquid chromatography with fluorescence detection

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, α-ergocryptine, ergocristine, ergonovine, and ergotamine. The average recovery was 61% ±?10% with limits of detection from 0.2 to 1.1 µg kg^?1. Twenty-four unknown rye flour samples from Danish mills contained on average 46 µg kg^?1 with a maximum content of 234 µg kg^?1. The most common ergot alkaloids were ergotamine and α-ergocryptine including their C8-isomers. A total of 54% of the ergot alkaloids were detected as C(8)-S isomers.     

Survey of fumonisins B1, B2 and B3 in conventional and organic retail corn products in Spain and Italy and estimated dietary exposure

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.     

Acrylamide–asparagine relationship in baked/toasted wheat and rye breads

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.     

Occurrence and intake of deoxynivalenol in cereal-based products marketed in Korea during 2007–2008

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.     

Simultaneous determination of type A,B and D trichothecenes and their occurrence in cereals and cereal products

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.     

Tropane and ergot alkaloids in grain-based products for infants and young children in the Netherlands in 2011–2014

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.     

Occurrence of pyrrolizidine alkaloids in animal- and plant-derived food: results of a survey across Europe

Pyrrolizidine alkaloids (PAs) are secondary metabolites of plant families such as Asteraceae or Boraginaceae and are suspected to be genotoxic carcinogens. Recent investigations revealed their frequent occurrence in honey and particularly in tea. To obtain a comprehensive overview of the PA content in animal- and plant-derived food from the European market, and to provide a basis for future risk analysis, a total of 1105 samples were collected in 2014 and 2015. These comprised milk and milk products, eggs, meat and meat products, (herbal) teas, and (herbal) food supplements collected in supermarkets, retail shops, and via the internet. PAs were detected in a large proportion of plant-derived foods: 91% of the (herbal) teas and 60% of the food supplements contained at least one individual PA. All types of (herbal) teas investigated were found to contain PAs, with a mean concentration of 460 µg kg^?1 dry tea (corresponding to 6.13 µg L^?1 in [herbal] tea infusion). The highest mean concentrations were found in rooibos tea (599 µg kg^?1 dry tea, 7.99 µg L^?1 tea infusion) and the lowest in camomile tea (274 µg kg^?1 dry tea, 3.65 µg L^?1 tea infusion). Occurrence of PAs in food supplements was found to be highly variable, but in comparable ranges as for (herbal) tea. The highest concentrations were present in supplements containing plant material from known PA-producing plants. In contrast, only 2% of the animal-derived products, in particular 6% of milk samples and 1% of egg samples, contained PAs. Determined levels in milk were relatively low, ranged between 0.05 and 0.17 µg L^?1 and only trace amounts of 0.10–0.12 µg kg^?1 were found in eggs. No PAs were detected in the other animal-derived products.     

Determination of tetracycline residues in chicken meat by liquid chromatography-tandem mass spectrometry

Analysis of residual levels of tetracyclines (TCs) in chicken meat was performed using a validated liquid chromatography coupled with a tandem mass spectrometry (LC-MS/MS) technique. Overall, the recoveries for TCs ranged from 56.9% to 101.2%, with standard deviations of 4.5–13.2%. Detection limits ranged from 7.9 to 14.6?µg?kg^?1. In four of 60 samples, doxycycline (DXC) was determined in a range from 19.9 to 35.6?µg?kg^?1; and in one sample tetracycline was detected at 17.2?µg?kg^?1. Chlortetracycline (CTC) and oxytetracycline (OTC) were not detected in any of the tested samples. This study indicates that chicken meat sold in Bursa, Turkey, contained some residues of TCs. Therefore, stricter regulations for the use of antibiotics in the poultry industry and the monitoring of drug residues in chicken meat prior to marketing are needed. Finally, this method has been applied successfully for the confirmation of TCs in chicken meat.     

Survey of levels of cadmium in oysters,mussels, clams and scallops from the Pacific Northwest coast of Canada

Field and retail collections of bivalves from the Pacific Northwest, Canada, were analysed for cadmium concentrations by atomic absorption spectrophotometry (AAS). Both collections of varnish (Nuttallia obscurata) and manila (Venerupis philippinarum) clams contained cadmium concentrations of less than 0.5 µg g^?1, well below international safety guidelines of 1 and 2 µg g^?1 wet weight cadmium for the European and Hong Kong markets, respectively, as well as the 2 µg g^?1 safety guideline set by the Codex Alimentarius Commission (CAC). Cadmium concentrations in retail collections of the Pacific oyster, Crassostrea gigas, were generally above 2 µg g^?1 wet weight (range = 1.5–3.56 µg g^?1). Retail collections of the mussel, Mytilus spp., contained cadmium concentrations below the 2 µg g^?1 wet weight guideline, but not always the 1 µg g^?1 limit (range = 0.15?1.8 µg g^?1). However, field collections of Mytilus spp. contained cadmium concentrations between 0.35 and 4.00 µg g^?1 wet weight, and depending on sampling location, concentrations exceeded the CAC guidelines by more than two-fold. Locations where mussels had high cadmium concentrations correlated with regions that had previously reported high values for cadmium in Pacific oysters (r = 0.65; p < 0.05). Of the various shellfish analysed, the four species of scallops, Chlamys hastata, C. rubida, Crassadoma gigantea, and Patinopecten yessoensis, contained the greatest concentrations of cadmium, in excess of 5 µg g^?1 wet weight (range = 4.97–8.98 µg g^?1) with the greatest concentrations determined for C. gigantea. Cadmium concentrations in shellfish from the Pacific Northwest are greater than values reported for shellfish from other regions of the world and consumers need be aware of Health Canada consumption guidelines for shellfish from this region.     

Exposure of consumers to morphine from poppy seeds in Hungary

Poppy seed-containing foods are popular dishes in Hungary and some other Central European countries. The alkaloids of poppy are used in the production of medicines. Poppy seeds used as food may also contain considerable amounts of alkaloids, which raises the question of food safety. Morphine, codeine, thebaine and noscapine concentrations of poppy seed samples from the period 2001–2010 and consumption data from two Hungarian surveys, carried out in 2003 and 2009, were evaluated. Exposure calculations were made for morphine intake by both point estimate and probabilistic methods, and the uncertainty of the calculated values was estimated. The point estimate for the acute consumer exposure, calculated using the 97.5th percentiles of morphine concentration and of poppy seed consumption and taking into account the reduction of morphine content by processing, was 78.64?µg (kg?bw)^?1 day^?1 for adults, and 116.90?µg (kg?bw)^?1?day^?1 for children. Based on probabilistic estimations, the 97.5th and 99th percentile exposures ranged between 18.3–25.4 and 25.6–47.4?µg (kg?bw)^?1?day^?1 for adults, and between 32.9 and 66.4?µg (kg?bw)^?1 day^?1 for children, respectively. As a no observed effect level (NOEL) had not been established, the significance of exposure could not be assessed.     

Lead concentration in meat from lead-killed moose and predicted human exposure using Monte Carlo simulation

Lead-based hunting ammunitions are still common in most countries. On impact such ammunition releases fragments which are widely distributed within the carcass. In Norway, wild game is an important meat source for segments of the population and 95% of hunters use lead-based bullets. In this paper, we have investigated the lead content of ground meat from moose (Alces alces) intended for human consumption in Norway, and have predicted human exposure through this source. Fifty-two samples from different batches of ground meat from moose killed with lead-based bullets were randomly collected. The lead content was measured by atomic absorption spectroscopy. The lead intake from exposure to moose meat over time, depending on the frequency of intake and portion size, was predicted using Monte Carlo simulation. In 81% of the batches, lead levels were above the limit of quantification of 0.03?mg?kg^?1, ranging up to 110?mg?kg^?1. The mean lead concentration was 5.6?mg?kg^?1, i.e. 56 times the European Commission limit for lead in meat. For consumers eating a moderate meat serving (2?g?kg^?1 bw), a single serving would give a lead intake of 11?µg?kg^?1 bw on average, with maximum of 220?µg?kg^?1 bw. Using Monte Carlo simulation, the median (and 97.5th percentile) predicted weekly intake of lead from moose meat was 12?µg?kg^?1 bw (27?µg?kg^?1 bw) for one serving per week and 25?µg?kg^?1 bw (45?µg?kg^?1 bw) for two servings per week. The results indicate that the intake of meat from big game shot with lead-based bullets imposes a significant contribution to the total human lead exposure. The provisional tolerable weekly intake set by the World Health Organization (WHO) of 25?µg?kg^?1 bw is likely to be exceeded in people eating moose meat on a regular basis. The European Food Safety Authority (EFSA) has recently concluded that adverse effects may be present at even lower exposure doses. Hence, even occasional consumption of big game meat with lead levels as those found in the present study may imply an increased risk for adverse health effects. Children and women of child-bearing age are of special concern due to the neurodevelopmental effects of lead.     

Identification and quantification of the migration of chemicals from plastic baby bottles used as substitutes for polycarbonate

The results of a study on the analytical identification and quantification of migration of chemicals from plastics baby bottles found in the European Union market made of materials that are now present as substitutes for polycarbonate (PC) are reported. A total of 449 baby bottles with a focus on first age or sets of bottles were purchased from 26 European Union countries, Canada, Switzerland and the USA. From this collection, which contained several duplicates, a total of 277 baby bottles were analysed. The materials included different types of plastic such as PC, polyamide (PA), polyethersulphone (PES), polypropylene (PP), but also silicone, and from the United States a co-polyester marketed under the trade name Tritan?. The bottles were subjected to the conventional migration test for hot fill conditions, i.e. 2?h at 70°C. The simulant used was that specified in European Union legislation (2007/19/EC) for milk, i.e. 50% ethanol. In a first phase 1, migration was conducted since the scope of this investigation was a screening rather than a true compliance testing check. Second and third migrations were performed on selected articles when migrated substances exceeded limits specified in the legislation. In order to verify some materials, a portion of the bottle was cut to run an FT-IR fingerprint to confirm the nature of the polymer. The migration solutions in general showed a low release of substances. Results showed that bottles made of PP and silicones showed a greater number of substances in the migration solutions and in greater quantity. Chemicals from PP included alkanes, which could be found in >65% of the bottles at levels up to 3500?µg?kg^?1; and benzene derivatives in 17% of the baby bottles and found at levels up to 113?µg?kg^?1. Some substances were found on a regular basis such as plasticisers, esters and antioxidants (e.g. tris(2,4-di-tert-butylphenyl)phosphate, known as Irgafos 168. Some substances found were not included in the Community positive list, which means that those should not be found even in the first migration. Such substances included 2,6-di-isopropylnaphthalene (DIPN), found in 4% of the bottles at levels up to 25?µg?kg^?1, 2,4-di-tert-butyl phenol (in 90% of the bottles at levels up 400?µg?kg^?1). Moreover, bisphenol A (BPA) was detected and quantified in baby bottles made of PA, but limited to one brand and model specific (but labelled BPA free). Results for baby bottles made of silicone also indicated the presence of components, e.g. potentially coming from inks (benzophenone, diisopropyl naphtahalene – DIPN, which could come for example from the presence of instruction leaflets in the bottles). In the case of silicone, phthalates were also found in relevant concentrations, with levels for DiBP and DBP from the first migration test of 50–150?µg?kg^?1 and DEHP at levels 25–50?µg?kg^?1.     

Immunoaffinity chromatography purification and ultra-high-performance liquid chromatography-tandem mass spectrometry determination of four β-agonists in beef

A highly selective and sensitive method was developed for the simultaneous determination of four β-agonists (clenbuterol, salbutamol, ractopamine and terbutaline) in beef by immunoaffinity chromatography purification coupled to ultra-high-performance LC-MS/MS. The MS/MS conditions, ultra-high-performance LC mobile phase, injection solution, sample purification process and matrix effect were studied to optimise the operation conditions. The limits of detection (LODs) of the instrument for the studied β-agonists ranged from 0.20 to 0.25?µg?l^?1, and the LODs of the method for the studied β-agonists ranged from 0.20 to 3.00?µg?kg^?1 for beef. Calibration curves were constructed using a standard solution diluted with blank beef matrix. The linear ranges of the calibration curves ranged from 5 to 100?µg?kg^?1 and the coefficients of determination were >0.9942 (n?=?10) for all four β-agonists. Samples spiked at 5, 10 and 50?µg?kg^?1 showed recoveries >72% and RSDs <6.6%. The method is suitable for the simultaneous detection of four β-agonists at trace levels in beef.     

Survey of aflatoxins in maize tortillas from Mexico City

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).     

Natural occurrence of type-B trichothecene mycotoxins in Korean cereal-based products

Type-B trichothecenes (deoxynivalenol (DON), nivalenol (NIV), fusarenone-X (FUS-X), 15-acetyldeoxynivalenol (15ADON), and 3-acetyldeoxynivalenol (3ADON)) were determined in 338 cereal-based products. Detection limit, quantification limit and mean recovery for five toxins were in the ranges 0.7–2.6?µg?kg^?1, 2.1–7.8?µg?kg^?1 and 73–110%, respectively. The range of occurrence and average level in samples were, respectively, 21–88% and 5.2–121.8?µg?kg^?1 for NIV, 10–96% and 1.7–109.5?µg?kg^?1 for DON, 2–39% and 0.4–3.6?µg?kg^?1 for FUS-X, 0–80% and 0–17.3?µg?kg^?1 for 15ADON, and 0–29% and 0–1.5?µg?kg^?1 for 3ADON. Regarding co-occurrence, 64% of samples had more than two type-B trichothecenes. The estimated daily intakes of NIV, DON, FUS-X, 15ADON, and 3ADON were 0.077, 0.048, 0.004, 0.006 and 0.002?µg?kg^?1?bw?day^?1, respectively. These results suggest that current exposure levels do not indicate the possibility of adverse effects, but consideration of the combined exposure of type-B trichothecenes may be required due to the high frequency of co-occurrence.     

Validation of a commercial receptor kit Sulfasensor® Honey for the screening of sulfonamides in honey according to Commission Decision 2002/657/EC

The Sulfasensor® Honey kit is a receptor test dedicated to the screening of sulphonamide residues respectively in different matrices. The aim of this project was to evaluate and validate this kit according to the Community Reference Laboratory (CRL) guideline for the validation of screening methods to achieve the French control plan for honey. The test is robust, quick (90?min for 40 samples), easy to perform and easy to read. The false-positive rate was estimated to be 12.5%. The detection capabilities CCβ of the kit were lower than or equal to 25?µg?kg^?1 for sulfamethazine, sulfamerazine, sulfathiazole and sulfapyridine, and between 25 and 50?µg?kg^?1 for sulfadiazine and sulfadimethoxine, 150?µg?kg^?1 for sulfaquinoxaline, and 1000?µg?kg^?1 for sulfamethoxazole and sulfamethizole. Sulfanilamide was not detected by the kit. The kit was applicable to a wide variety of honeys (different floral and geographical origins, liquid or solid). This kit was used to implement the French control plan for the detection of antibiotic residues in honey in 2010 in parallel with an HPLC method. However, in 2011 the kit was replaced by an LC-MS/MS method for the screening and confirmation of sulfonamide residues in honey, which detects all the sulfonamides of interest.     

Comparison of methods and optimisation of the analysis of fumonisins B1 and B2 in masa flour,an alkaline cooked corn product

A comparison study of different extraction and clean-up procedures for the liquid chromatographic analysis of fumonisins B₁ (FB₁) and B₂ (FB₂) in corn masa flour was performed. The procedures included extraction (heat or room temperature) with acidic conditions or EDTA-containing solvents, and clean-up by immunoaffinity or C18 solid-phase extraction columns. Thereafter an analytical method was optimised using extraction with an acidic mixture of methanol–acetonitrile–citrate/phosphate buffer, clean-up through the immunoaffinity column and determination of fumonisins by liquid chromatography with automated pre-column derivatisation with o-phthaldialdehyde reagent. Recovery experiments performed on yellow, white and blue masa flours at spiking levels of 400, 800 and 1200?µg?kg^?1 FB₁ and of 100, 200 and 300?µg?kg^?1 FB₂ gave overall mean recoveries of 99% (±6%) for FB₁ and 88% (±6%) for FB₂. Good recoveries (higher than 90% for both FB₁ and FB₂) were also obtained with corn tortilla chips. The limits of quantification of the method (signal-to-noise ratio of 10) were 25?µg?kg^?1 for FB₁ and 17?µg?kg^?1 for FB₂. The method was tested on different commercial corn masa flours as well as on white and yellow corn tortilla chips, showing fumonisin contamination levels (FB₁?+?FB₂) up to 1800?µg?kg^?1 (FB₁?+?FB₂) in masa flour and 960?µg?kg^?1 in tortilla chips. Over 30% of masa flours originating from Mexico exceeded the European Union maximum permitted level.     

Evaluation and validation of two microbiological tests for screening antibiotic residues in honey according to the European guideline for the validation of screening methods

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%.     

Genetic variation in the extract viscosity of rye (Secale cereale L.) bread made from endosperm and wholemeal flour: impact of high-molecular-weight arabinoxylan, starch and protein

BACKGROUND: To verify the viscous potential of rye bread made from population and hybrid cultivars, the overall extract viscosities (EVs) of endosperm and wholemeal breads (EBs and WMBs respectively) were assessed using extractants of different pH. Also, arabinoxylan‐dependent EV (AX‐EV) was determined after combined action of starch‐ and protein‐degrading enzymes. RESULTS: The synergistic effect of a combination of α‐amylase, amyloglucosidase and protease on EV was almost two times higher than the effects observed after single addition of each of them. However, water‐extractable arabinoxylans (WE AXs) were the major contributors to EV. Unexpectedly, a decrease in the mean WE AX contents observed in the following order, WMB (31.7 g kg^?1) and EB (29.3 g kg^?1) of hybrid rye and WMB (28.8 g kg^?1) and EB (23.8 g kg^?1) of population rye, was accompanied by an increase in their AX‐EVs (12, 21, 21 and 29 mPa s respectively). CONCLUSION: In some cases the structure of WE AXs is a more important determinant of AX‐EV than their content in rye bread. Nevertheless, both factors influence AX‐EV, which may reflect the viscosity of the human small intestine after rye bread consumption, related to some beneficial metabolic effects. Therefore AX‐EV can be a preliminary parameter for selection towards high‐viscosity bread. Copyright © 2010 Society of Chemical Industry