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A Boenke

Publications and source records attributed to A Boenke.

28 records · Page 2Linked to original sources

Deoxynivalenol in wheat and maize flour reference materials. 2. Preparation and certification.

The preparation of four cereal reference materials (two wheat and two maize) and the certification of their 4-deoxynivalenol (DON) contents is described. The materials were prepared and certified within the BCR programme of the Commission of the European Community as part of a broad activity to improve accuracy and agreement of measurements of importance in food and agriculture. Reference material RM 379 was prepared from naturally contaminated wheat four blended with 'blank' material to achieve the desired DON content. The reference material RM 378 was prepared from naturally contaminated maize identified as containing approximately the desired DON content. Details are given of the milling, blending and packaging procedure, and the checks to ensure homogeneity and stability of the materials. The reference materials RM 396 and 377 were similarly prepared from the blank wheat and maize samples respectively. The certification exercise was carried out by five laboratories (with a further two to three laboratories providing supporting data) using a variety of extraction and clean-up procedures with either high performance liquid chromatography (HPLC) or gas chromatography (GC) as the determinative stages. Wheat RM 379 was certified as containing DON at a level of 673 +/- 21 micrograms/kg and wheat RM 396 as containing less than 50 micrograms/kg. Maize RM 378 was certified as containing DON at 425 +/- 38 micrograms/kg and maize RM 377 as containing less than 50 micrograms/kg. The materials are intended for the verification of methods used to determine DON in cereal samples.

Certification↗

Ochratoxin A in wheat: an intercomparison of procedures.

The Commission of the European Communities' Community Bureau of Reference (BCR) has undertaken a project to improve methodology and to prepare suitable certified reference materials in order to provide a basis for analytical quality control for the determination of ochratoxin A. The first phase of the project, an intercomparison of procedures for the determination of ochratoxin A in wheat at a level of approximately 13 micrograms/kg, is described. The study involved 24 European laboratories which analysed a naturally contaminated wheat and a 'blank' wheat sample (ochratoxin A content < 1 microgram/kg). The participants used a variety of procedures, including chloroform, methanol, toluene and ethyl acetate for extraction, and silica-, reversed phase- and immunoaffinity columns for clean-up. HPLC (one laboratory used TLC) was applied as the determinative step. Several performance characteristics were checked and the ochratoxin A content was determined. Recoveries were found to range from 25 to 100%. The coefficient of variation from all the results calculated on the basis of peak height was 23%. The study showed that the variation of results was influenced more by the clean-up step than by the extraction solvent. Some laboratories suffered significant day-to-day effects while others found difficulties with interfering peaks in the 'blank' material. It is planned for the next study to improve the recovery range, the clean-up step and the reproducibility (within-laboratory, between-days) and to check the influence of co-extractives from the matrix.

Chromatography, High Pressure Liquid↗

Stability of fumonisins (FB1 and FB2) in solution.

The stability of fumonisins B1 and B2 (FB1 and FB2) during 6 week storage was studied in acetonitrile:water (1:1) and methanol at four storage temperatures (-18, 4, 25 and 40 degrees C). Samples were analysed by HPLC with fluorescence detection after derivatization with o-phthaldialdehyde. Decomposition of fumonisins was evident in a methanol solution after 6 week storage at 4, 25 and 40 degrees C (signals for both toxins decreased by 5, 35 and 60%, respectively), whereas no losses were observed in samples stored at -18 degrees C. Both fumonisins were quite stable in acetonitrile:water solution at any of the four storage temperatures. The stability of fumonisins in acetonitrile:water (1:1) was confirmed over a period of 6 months at three temperatures (-18, 4 and 25 degrees C) in two solutions at different mass concentrations. No significant difference (t0.95-test) was observed between solutions stored in the dark at different temperatures and for different times (3 and 6 months). The overall coefficient of variation (n = 24, four measurements at each storage time and temperature) in each solution was < 3% for both toxins. Acetonitrile:water (1:1), unlike methanol, is a suitable solvent for fumonisin reference solutions.

Acetonitriles↗

The development of five animal feed reference materials, certified for their aflatoxin B1 content.

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.

Aflatoxin B1↗

Beta-agonists in animal feed. IV: Intercomparison study of a candidate reference confirmatory method.

The objective of this intercomparison study was to evaluate the qualitative aspects and the interlaboratory performance of the method selected to be recommended as the official Community reference confirmatory method for the analysis of beta-agonists in animal feed. This method contains three possible options, i.e. a narrow range method for clenbuterol-type compounds based either on HPLC or on GCMS as the end-determination step and a broad range GCMS method for clenbuterol-type and salbutamol-type-beta-agonists. Three types of animal feed materials were provided: a series of blank materials and two series of materials contaminated with clenbuterol and salbutamol at a low and a high level, respectively. The results showed that the majority of the laboratories were able to identify blank, low and high level materials both for clenbuterol and salbutamol. For clenbuterol the narrow range GCMS method has been shown to be the most satisfactory. Although the participants had comments on the purity of the extracts obtained by means of the broad range method it was found appropriate as a multi-residue method which is able to measure simultaneously clenbuterol-type and salbutamol-type beta-agonists. A statistical evaluation of the quantitative measurement was also performed.

Adrenergic beta-Agonists↗

European intercomparison study for the determination of the fumonisins content in two maize materials.

The results of an intercomparison study for the analysis of fumonisin B1 (FB1) and fumonisin B2 (FB2) in a contaminated maize material (Maize B, containing approximately 2 micrograms/g FB1 and 1 micrograms/g FB2) and its 'blank' counterpart (Maize A, containing less than 20 ng/g FB1 and FB2) are reported. Maize materials were distributed in 60 g sachets, submitted to gamma-irradiation at 15 kGy, and distributed to participating laboratories. The study was carried out by 24 European laboratories, most of which have national or international responsibilities for food/feed quality control. Participants used basically one method with some modifications, based on clean-up through SAX minicolumn and reversed phase HPLC with fluorescence detection of the OPA-fumonisin derivatives. The intercomparison study generated data (after correction for recoveries) with repeatability and reproducibility levels of: RSDr = 10% and RSDR = 11% for FB1; RSDr = 11% and RDSR = 13% for FB2. The recoveries obtained by most participants were considered low (70% for FB1 and 69% for FB2), being considerably affected by the extraction mode. Average recoveries for laboratories using blending were 62% and 60%, whereas for laboratories using shaking they were 85% and 86% for FB1 and FB2, respectively. The day-to-day- data showed a between-day, within-laboratory repeatability lower than 15% (CV < 15%) for FB1 for all laboratories, whereas only three laboratories obtained a between-day, within-laboratory reproducibility higher than 15% (CV > 15%) for FB2.

Animal Feed↗

Stability of fumonisins at different storage periods and temperatures in gamma-irradiated maize.

The effect of gamma-irradiation on fumonisin B1 (FB1) and fumonisin B2 (FB2) occurring in maize materials has been investigated together with the stability of fumonisins in gamma-irradiated maize stored at different temperatures (-18 to +40 degrees C) for different periods (2, 4, 13 and 26 weeks). Fifteen KGy gamma-irradiation was required to sterilize efficiently maize flour. This process caused a decrease in fumonisin content of about 20%. The stability studies showed that fumonisins are stable in gamma-irradiated maize for at least 6 months at 25 degrees C or at least 4 weeks at 40 degrees C. These data indicate that gamma-irradiation is an appropriate technique for obtaining sterilized maize materials to be used for intercomparison studies on analytical procedures for the measurement of the fumonisin content.

Carboxylic Acids↗

Activities and current research from the EC, standards, measurements and testing programme (SMT) in the area of food contact materials.

The EC, Standards, Measurements and Testing Programme (SMT) is the successor of the Measurements and Testing Programme (M&T) and the Community Bureau of Reference (BCR). Its objectives include the provision of research and technical support to standardization and health of the society when it is required to improve the competitive position of European industry, and for the development or implementation of Community policy. The SMT-Programme is currently supporting a number of different types of collaborative projects in the food packaging sphere. Their objectives range from method development via preparation and certification of reference materials, preparation of a handbook and the update of a spectral atlas to pre-normative research providing information on a number of sources and wide range of packed products being transported throughout Europe.

European Union↗

Sampling plans for the determination of aflatoxin B1 in large shipments of animal feedstuffs.

Incremental samples (50, 100, and 500 g) were systematically collected from large shipments of copra meal pellets, copra cake, and palm kernel cake to study the distribution of aflatoxin B1 and evaluate adherence of distribution to the model, CV(2)is (EQ) = A + B/Mis (where CVis = coefficient of variation of the true concentration of aflatoxin B1 within the incremental samples; Mis = mass of the incremental samples; and A and B are constants). Also evaluated was the distribution of aflatoxin B1 among 1 kg composite samples, produced both by random combination of existing incremental samples and by collection of 1 kg composite samples (composed of 10 x 100 g increments) from additional batches of copra meal pellets and cottonseed cake. The efficiency of selected sample preparation (grinding and subdivision) procedures was compared, culminating in the development and description of a variety of sampling plans. The coefficient of variation (CV) among incremental samples varied from 0 to 38%, and was independent of incremental sample size. No significant difference (F-test, 5% significance level) was found between the efficacy of 4 sample preparation methods when these methods were applied to the commodities described above. Various sampling plans were evaluated with estimated CVs from 4.0 to 12.5%, for the aflatoxin B1 content of the composite samples.

Aflatoxin B1↗

Development of reference materials for paralytic shellfish poisoning toxins.

A project was undertaken to develop mussel reference materials that were certified for their mass fractions of saxitoxin and decarbamoyl-saxitoxin. Fifteen laboratories from various European countries participated. Three of these had major responsibility for substantial parts of the work and overall coordination of the project. The project involved 4 main activities: (1) procurement and characterization of calibrants; (2) improvement of analytical methodology; (3) preparation of reference materials, including homogeneity and stability studies; (4) 2 interlaboratory studies and a certification exercise. The joint activities resulted in 3 homogeneous and stable reference materials: 2 lyophilized mussel materials with and without naturally incurred paralytic shellfish poisoning (PSP) toxins, and a saxitoxin enrichment solution. The reference materials were certified with respect to their saxitoxin and decarbamoyl-saxitoxin content. The lyophilized mussel material with PSP toxins (CRM 542) contained <0.07 mg saxitoxin x 2HCl/kg and 1.59 +/- 0.20 mg decarbamoyl-saxitoxin x 2HCl/kg. The lyophilized mussel material without PSP toxins (CRM 543) contained <0.07 mg saxitoxin x 2HCl/kg and <0.04 mg decarbamoyl-saxitoxin x 2HCl/kg. The certified value of the saxitoxin mass fraction in the saxitoxin enrichment solution (CRM 663) was 9.8 +/- 1.2 microg/g.

Animals↗