Survey of moniliformin in wheat- and corn-based products using a straightforward analytical method

A straightforward analytical method was developed and validated to determine the mycotoxin moniliformin in cereal-based foods. Moniliformin is extracted with water and quantified with liquid chromatography tandem mass spectrometry, and its presence confirmed with liquid chromatography-Orbitrap-high-resolution mass spectrometry. The method was validated for flour, bread, pasta and maize samples in terms of linearity, matrix effect, recovery, repeatability and limit of quantification. Quantification was conducted by matrix-matched calibration. Positive samples were confirmed by standard addition. Recovery ranged from 77 to 114% and repeatability from 1 to 14%. The limit of quantification, defined as the lowest concentration tested at which the validation criteria of recovery and repeatability were fulfilled, was 10 µg/kg. The method was applied to 102 cereal-based food samples collected in the Netherlands and Germany. Moniliformin was not detected in bread samples. One of 22 flour samples contained moniliformin at 10.6 µg/kg. Moniliformin occurred in seven out of 25 pasta samples at levels around 10 µg/kg. Moniliformin (MON) was present in eight out of 23 maize products at levels ranging from 12 to 207 µg/kg

Identification of clastogenic and/or aneugenic events during the preneoplastic stages of experimental rat hepatocarcinogenesis by fluorescence in situ hybridization

A growing body of evidence from human and animal cancer cytogenetics studies indicates that aneuploidy is an important chromosome change in carcinogenesis. To understand the role of this genetic phenomenon during the first steps of an experimental cancer model, molecular and cellular techniques were combined. A sequential cytogenetic study of a modified Solt-Farber liver cancer model in the rat was performed to identify the importance of chromosome versus genome mutations. Male Wistar rats were initiated with diethylnitrosamine (DENA), followed by a 2-acetylaminofluorene exposure to select resistant hepatocytes. Chronic phenobarbital (PB) treatment was used to induce promotion. Cell proliferation was induced by a necrogenic dose of CCl4, administered during the selection period (Gerlans protocol) or 3 days before hepatocyte isolation (experimental protocol). In order to discriminate between genetic events causing chromosome breakage (clastogenic) and those that induce chromosome loss (aneugenic), isolated micronucleated hepatocytes (MNH) were analysed for the presence of a centromere in the micronucleus (MN). Non-radioactive in situ hybridization with a rat centromere satellite 1 DNA probe was applied. Our results show that the majority of the observed genetic changes, expressed as MN during different preneoplastic stages, were of clastogenic origin. However, the number of induced aneugenic hepatocytes increased markedly during the promotion period of the Gerlans protocol (~7-fold above control) and during PB exposure in the experimental protocol (~4-fold above control). Additionally, these stages were also characterized by an increased level of MN expression (20.3 < ?MNH < 32.8), in comparison with the initiation stage after DENA exposure (13.5 < ?MNH < 17.1). Although it is not yet clear if these genetic alterations have a causative nature in neoplastic liver transformation, the use of interphase cytogenetics certainly might lead to a better understanding of the genomic changes which occur during experimental hepatocarcinogenesis.SCOPUS: ar.jinfo:eu-repo/semantics/publishe

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

Fate of enniatins and deoxynivalenol during pasta cooking

The fate of deoxynivalenol and enniatins was studied during cooking of commercially available dry pasta in the Netherlands in 2014. Five samples containing relatively high levels of deoxynivalenol and/or enniatins were selected for the cooking experiment. Cooking was performed in duplicate on different days, under standardised conditions, simulating house-hold preparation. Samples were extracted with a mixture of acetonitrile/water followed by salt-induced partitioning. The extracts were analysed by LC–MS/MS. The method limits of detection were 8 μg/kg for deoxynivalenol, 10 μg/kg for enniatin A1 and 5 μg/kg for enniatins A, B and B1. During the cooking of the five dry pasta samples, 60% of the deoxynivalenol and 83–100% of the enniatins were retained in the cooked pasta. It is recommended to study food processing fate of mycotoxins through naturally contaminated materials (incurred materials)

Simultaneous quantification of ergot and tropane alkaloids in bread in the Netherlands by LC-MS/MS

Atropine and scopolamine are tropane alkaloids (TAs), which are regulated for cereal-based foods for children in the EU. For ergot alkaloids (EAs) in cereals and cereal-based food harmonised legislation is not yet established. A fast and straightforward method, which employs extraction by acidified water/methanol followed by ultra-filtration prior to analysis by LC-MS/MS, was validated in bread for 20 EAs and six TAs. LOQs for individual alkaloids ranged from 0.3 to 1.2 µg kg−1, while recoveries ranged from 65% to 94% and repeatability from 3.4% to 17%. A survey was conducted in the Netherlands on 40 retail samples of bread (wheat, rye, wheat-rye, multi-grain) collected in 2014 and 2018. TAs, including atropine and scopolamine, were not detected. Eighteen different EAs were detected and total levels varied between −1. Since EAs were detected in a wide concentration range, it is recommended to monitor their occurrence in bread more regularly.</p

Survey of moniliformin in wheat- and corn-based products using a straightforward analytical method

A straightforward analytical method was developed and validated to determine the mycotoxin moniliformin in cereal-based foods. Moniliformin is extracted with water and quantified with liquid chromatography tandem mass spectrometry, and its presence confirmed with liquid chromatography-Orbitrap-high-resolution mass spectrometry. The method was validated for flour, bread, pasta and maize samples in terms of linearity, matrix effect, recovery, repeatability and limit of quantification. Quantification was conducted by matrix-matched calibration. Positive samples were confirmed by standard addition. Recovery ranged from 77 to 114% and repeatability from 1 to 14%. The limit of quantification, defined as the lowest concentration tested at which the validation criteria of recovery and repeatability were fulfilled, was 10 μg/kg. The method was applied to 102 cereal-based food samples collected in the Netherlands and Germany. Moniliformin was not detected in bread samples. One of 22 flour samples contained moniliformin at 10.6 μg/kg. Moniliformin occurred in seven out of 25 pasta samples at levels around 10 μg/kg. Moniliformin (MON) was present in eight out of 23 maize products at levels ranging from 12 to 207 μg/kg

Straightforward analytical method to determine opium alkaloids in poppy seeds and bakery products

A straightforward method to determine the content of six opium alkaloids (morphine, codeine, thebaine, noscapine, papaverine and narceine) in poppy seeds and bakery products was developed and validated down to a limit of quantification (LOQ) of 0.1 mg/kg. The method was based on extraction with acetonitrile/water/formic acid, ten-fold dilution and analysis by LC-MS/MS using a pH 10 carbonate buffer. The method was applied for the analysis of 41 samples collected in 2015 in the Netherlands and Germany. All samples contained morphine ranging from 0.2 to 240 mg/kg. The levels of codeine and thebaine ranged from below LOQ to 348 mg/kg and from below LOQ to 106 mg/kg, respectively. Sixty percent of the samples exceeded the guidance reference value of 4 mg/kg of morphine set by BfR in Germany, whereas 25% of the samples did not comply with the limits set for morphine, codeine, thebaine and noscapine by Hungarian legislation.</p

Straightforward analytical method to determine opium alkaloids in poppy seeds and bakery products

A straightforward method to determine the content of six opium alkaloids (morphine, codeine, thebaine, noscapine, papaverine and narceine) in poppy seeds and bakery products was developed and validated down to a limit of quantification (LOQ) of 0.1 mg/kg. The method was based on extraction with acetonitrile/water/formic acid, ten-fold dilution and analysis by LC-MS/MS using a pH 10 carbonate buffer. The method was applied for the analysis of 41 samples collected in 2015 in the Netherlands and Germany. All samples contained morphine ranging from 0.2 to 240 mg/kg. The levels of codeine and thebaine ranged from below LOQ to 348 mg/kg and from below LOQ to 106 mg/kg, respectively. Sixty percent of the samples exceeded the guidance reference value of 4 mg/kg of morphine set by BfR in Germany, whereas 25% of the samples did not comply with the limits set for morphine, codeine, thebaine and noscapine by Hungarian legislation.</p