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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (6)
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- 4.1 Biologische Materialschädigung und Referenzorganismen (1)
- 4.2 Material-Mikrobiom Wechselwirkungen (1)
Eingeladener Vortrag
- nein (5)
Deoxynivalenol (DON), nivalenol (NIV) and zearalenone (ZEN) are toxic secondary metabolites produced by several species of Fusarium fungi. These mycotoxins are often found together in a large variety of cereal-based foods, which are regulated by maximum content levels of DON and ZEN. To date, suitable certified reference materials (CRM) intended for quality control purposes are lacking for these Fusarium mycotoxins. In order to overcome this lack, the first CRM for the determination of DON, NIV and ZEN in naturally contaminated wheat flour (ERM®-BC600) was developed in the framework of a European Reference Materials (ERM®) project. This article describes and discusses the whole process of ERM®-BC600 development, including material preparation, homogeneity and stability studies, and an interlaboratory comparison study for certification. A total of 21 selected expert laboratories from different European countries with documented expertise in the field of mycotoxin analysis took part in the certification study using various gas and liquid chromatographic methods. The certified values and their corresponding expanded uncertainties (k=2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows: 102±11 µgkg-1 for DON, 1000±130 µgkg-1 for NIV and 90±8 µgkg-1 for ZEN.
Stable isotope dilution assay for the accurate determination of mycotoxins in maize by UHPLC-MS/MS
(2012)
A fast, easy-to-handle and cost-effective analytical
method for 11 mycotoxins currently regulated in maize and
other cereal-based food products in Europe was developed
and validated for maize. The method is based on two extraction
steps using different acidified acetonitrilewater mixtures.
Separation is achieved using ultrahigh-performance
liquid chromatography (UHPLC) by a linear watermethanol
gradient. After electrospray ionisation, tandem mass spectrometric
detection is performed in dynamic multiple reaction
monitoring mode. Since accurate mass spectrometric quantification
is hampered by matrix effects, uniformly [13C]-
labelled mycotoxins for each of the 11 compounds were added
to the sample extracts prior to UHPLC-MS/MS analysis.
Method performance parameters were obtained by spiking
blank maize samples with mycotoxins before as well as after
extraction on six levels in triplicates. The twofold extraction
led to total recoveries of the extraction steps between 97%and
111% for all target analytes, including fumonisins. The [13C]-
labelled internal standards efficiently compensated all matrix
effects in electrospray ionisation, leading to apparent recoveries
between 88% and 105% with reasonable additional costs.
The relative standard deviations of the whole method were
between 4% and 11% for all analytes. The trueness of the
method was verified by the measurement of several maize test
materials with well-characterized concentrations. In conclusion,
the developed method is capable of determining all
regulated mycotoxins in maize and presuming similar
matrix effects and extraction recovery also in other cerealbased
foods.
Die zuverlässige Überwachung geltender Mykotoxin-Grenzwerte ist elementarer Bestandteil von Lebensmittelsicherheit und Verbraucherschutz. Durch die zunehmende Bedeutung der Qualitätssicherung ist auch die Nachfrage an zertifizierten Referenzmaterialien (ZRM) in den letzten Jahren deutlich gestiegen. Dem steht derzeit jedoch nur eine sehr begrenzte Auswahl geeigneter ZRM gegenüber.
Mycotoxins are important non-anthropogenic food and feed contaminants, which can be present on almost every agricultural commodity. Effective consumer protection therefore essentially depends on food surveillance by reliable quantitative analysis enabled by appropriate quality control. Certified (matrix) reference materials (CRMs) are versatile tools to support Quality assurance. However, in the case of ochratoxin A (OTA), a hepato- and nephrotoxic mycotoxin, which is regulated in various foods, there is a lack of suitable CRMs. This lack has now been overcome by the development of two European Reference Materials (ERM®) for the Determination of OTA in roasted coffee (ERM®-BD475) and red wine (ERM®-BD476). This article discusses the material preparation process as well as the results of homogeneity and stability testing. Furthermore, the results of the inhouse certification studies carried out at BAM Federal Institute for Materials Research and Testing are presented and discussed. Interlaboratory comparison studies involving selected expert laboratories with documented Expertise in the field of mycotoxin analysis were conducted to confirm the certified values determined by BAM. The certified ochratoxin A values and their corresponding expanded uncertainties (k = 2) were assigned in full compliance with the requirements of ISO Guide 35 and are as follows:
(6.0 ± 0.6) µg kg-1 for roasted coffee, ERM®-BD475, and (0.52 ± 0.11) µg L-1 for red wine, ERM®-BD476.
rac-2,3-Dibromopropionamide
(2013)
The racemic title compound, C3H5Br2NO, was crystallized from methanol. In the crystal, adjacent molecules are linked through N–H···O hydrogen bonds, forming chains along the c-axis direction. These chains are linked through N–H···O hydrogen bonds, forming an undulating two-dimensional network lying parallel to the bc plane. There are also short Br···Br contacts present [3.514 (3) Å].
Ergotaminine
(2012)
The title compound {systematic name: (6aR,9S)-N-[(2R,5S,10aS,10bS)-5-benzyl-10b-hydroxy-2-methyl-3,6-dioxooctahydro-8H-oxazolo[3,2-a]pyrrolo[2,1-c]pyrazin-2-yl]-7-methyl-4,6,6a,7,8,9-hexahydroindolo[4,3-fg]quinoline-9-carboxamide}, C33H35N5O5, was formed by an epimerization reaction of ergotamine. The non-aromatic ring (ring C of the ergoline skeleton) directly fused to the aromatic rings is nearly planar [maximum deviation = 0.317 (4) Å] and shows an envelope conformation, whereas ring D, involved in an intramolecular N–H···N hydrogen bond exhibits a slightly distorted chair conformation. The structure displays chains running approximately parallel to the diagonal of bc plane that are formed through N–H···O hydrogen bonds.
The title compound, also known as cis-zearalenone (cis-ZEN), C18H22O5, has already been reported elsewhere [Griffin et al. (1981). ACA Ser. 29, 35], but no atomic coordinates are publicly available. The molecule is of interest with respect to its toxicity. In the crystal, intramolecular O—H···O hydrogen bonds stabilize the molecular conformation, while intermolecular O—H···O hydrogen bonds link the molecules to form infinite chains along the [110] and [1¯10] directions. The absolute configuration has been assigned by reference to an unchanging chiral centre in the synthetic procedure.