Chemische Charakterisierung und Spurenanalytik
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Demonstrating competency and equivalence for the measurement capacity of contaminants and nutrients in primary foodstuffs is a priority of the OAWG 10-year strategy for Track A core comparisons. Such measurements have posed significant challenges for reference material producers and calibration service providers. This key comparison (KC), under the topic of “non- polar analyte in high carbohydrate food matrix: trans-Zearalenone (trans-ZEN) in maize powder” , was a sector of the model system selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to demonstrate the Calibration and Measurement Capabilities (CMCs) of national metrology institutes (NMIs) and designated institutes (DIs).
17 NMIs and DIs participated in the Track A KC CCQM- 168 “non-polar analyte in high carbohydrate food matrix: trans-ZEN in maize powder” . Participants were requested to evaluate the mass fraction (μg/kg) of trans-ZEN in maize powder material. Methods like liquid-liquid extraction and SPE were applied in the pre-treatment, and HPLC-MS/MS and HPLC-FLD were used for detection by the participants. The mass fractions for trans-ZEN were in the range of (91.8 to 169) μg/kg with standard uncertainties of (1.5 to 24.7) μg/kg, and corresponding relative standard uncertainties from 1.5% to 14.6%. Two labs, INTI and BAM were excluded from the KCRV evaluation. INTI result was identified as an outlier and confirmed their method had insufficient specificity. For BAM the calibration approach they used does not meet the CIPM traceability requirements. The other 15 labs included in the calculation of the consensus KCRV all agreed within their standard uncertainties. Hierarchical Bayes was used as estimators in calculating KCRV and standard uncertainty.
Successful participation in CCQM-K168 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 1 μg/kg to 1000 μg/kg in a high carbohydrate food matrix.
Ergot alkaloids form a toxicologically relevant group of mould toxins (mycotoxins) that are among the most common contaminants of food and animal feed worldwide. Reliable controls are essential to minimise health risks and economic damage. Due to their toxicological relevance, EU limit values for 12 priority ergot alkaloids have been introduced for the first time in 2022 and range from 500 µg/kg in rye milling products down to 20 ug/kg Processed cereal-based foods for infants and young children[1]. High-performance liquid chromatography - mass spectrometry is used to quantify low concentrations of ergots in food, however the European standard analytical procedure cannot be applied due to the lack of isotopically labelled reference standards.
The complex structure of the ergot alkaloids makes a total synthesis extremely challenging, expensive and time-consuming. Therefore, we are focusing on different semi-preparative methods (electrochemistry, organic synthesis, heterogeneous catalysis) to specifically N-demethylate the C8 carbon atom of the lysergic acid moiety. The norergot alkaloid formed is then isotopically labelled using an electrophilic methyl source, i.e. iodomethane or dimethyl sulphate to obtain the specific isotopic labelled ergot alkaloid. Initial experiments have shown that N-demethylation of the ergot alkaloid ergotamine is possible by both electrochemical and wet-chemical organic synthesis. The next step is to adapt the previously determined reaction conditions to enable the synthesis of norergotamine on a mg scale.
Safe food is a prerequisite for good human health, however currently almost one in ten people in the world fall ill after eating contaminated food. National food safety authorities need to be able to manage food safety risks along the entire food chain. The Official Controls Regulation (EU) 2017/625 was put in place to ensure that food and feed law stipulates the need for validated analytical methods. However, whilst method development for food control and proficiency testing are well established by European Union Reference Laboratories and National Reference Laboratories, validation of the measurements involved, certified reference materials and internationally recognised calibration and measurement capabilities are currently often (?) lacking. This may erode trust in the accuracy of the measurements.
This poster presents Food-MetNet, a coordinated preparatory initiative to establish the European Metrology Network for Safe and Sustainable Food, recently approved by the European Association of National Metrology Institutes (EURAMET). Food-MetNet aims to establish an ongoing dialogue between the metrology community, reference laboratories and regulatory bodies, in order to (i) identify stakeholders’ needs, (ii) develop a sustainable knowledge-sharing programme and web-based platform for stakeholders and (iii) develop roadmaps and a strategic research agenda. Improved access to more reliable and accurate food safety measurements will enable reference laboratories to more confidently and effectively compare their measurement results and support accreditation. This is particularly important where national food safety authorities need to assess potential new contaminants, novel food ingredients and newly emerging food risks, and new measurements methods may be required as well as input into new documentary standards. The activities for sustainable food intend to boost the activity within the "EU green deal framework" to reduce food waste and losses, and the development of standards and methods that allow for the reuse of food waste. The support to new business opportunities and innovation will allow increasing the market competitiveness of EU food industries and the valorisation of waste by reducing environmental impacts.
This paper describes Food-MetNet, a coordinated preparatory initiative to establish the European Metrology Network on Food Safety (EMN-FS). Food-MetNet aims to establish a long-term ongoing dialogue between the metrology community and relevant stakeholders, in particular, European Union Reference Laboratories (EURLs), National Reference Laboratories (NRLs) and the Joint Research Centre (JRC). This dialogue is meant to support the collection of needs from stakeholders, the take-up of metrological research output and the development of the roadmaps needed to navigate future research.
The CCQM-K148.a comparison was coordinated by the BIPM on behalf of the CCQM Organic Analysis Working Group for NMIs and DIs which provide measurement services in organic analysis under the CIPM MRA. It was undertaken as a "Track A" comparison within the OAWG strategic plan. CCQM-K148.a demonstrates capabilities for assigning the mass fraction content of a solid organic compound having moderate molecular complexity, where the compound has a molar mass in the range (75 - 500) g/mol and is non-polar (pKow < −2), when present as the primary organic component in a neat organic solid and where the mass fraction content of the primary component in the material is in excess of 950 mg/g.
Participants were required to report the mass fraction of Bisphenol A present in one supplied unit of the comparison material. Participants using a mass balance method for the assignment were also required to report their assignments of the impurity components present in the material. Methods used by the seventeen participating NMIs or DIs were predominantly based on either stand-alone mass balance (summation of impurities) or qNMR approaches, or the combination of data obtained using both methods. The results obtained using thermal methods based on freezing-point depression methods were also reported by a limited number of participants. There was excellent agreement between assignments obtained using all three approaches to assign the BPA content.
The assignment of the values for the mass fraction content of BPA consistent with the KCRV was achieved by most of the comparison participants with an associated relative standard uncertainty in the assigned value in the range (0.1 - 0.5)%.
The demonstration of competency and equivalence for the assessment of levels of contaminants and nutrients in primary foodstuffs is a priority within the 10-year strategy for the OAWG Track A core comparisons. The measurements are core challenges for reference material producers and providers of calibration Services. This key comparison related to low polarity analytes in a high fat, low protein, low carbohydrate food matrix and Benzo[a]pyrene in edible oil was the model System selected to align with this class within the OAWG strategy. Evidence of successful participation in formal, relevant international comparisons is needed to document measurement capability claims (CMCs) made by national metrology institutes (NMIs) and designated institutes (Dis). 16 National Metrology Institutions participated in the Track A Key Comparison CCQM-K146 Low-Polarity Analyte in high fat food: Benzo[a]pyrene in Olive Oil. Participants were requested to evaluate the mass fractions, expressed in µg/kg, of Benzo[a]pyrene in the olive oil material. The KCRV was determined from the results of all NMIs/DIs participating in the key comparison that used appropriately validated methods with demonstrated metrological traceability. Different methods such as liquid-liquid extraction, GPC and SPE were applied in the sample pretreatment and HPLC-FLD, HPLC-MS/MS, and GC-MS or GC-MS/MS were applied for detection by the participants. The mass fractions for BaP were in the range of (1.78 to 3.09) µg/kg with Standard uncertainties of (0.026 to 0.54) µg/kg, with corresponding relative Standard uncertainties from 0.9% to 21%. Five labs withdrew their result from the Statistical evaluation of the KCRV for technical reasons. One lab was excluded from the KCRV evaluation, as they did not meet the CIPM metrological traceability requirements. A Hierarchical Bayes option was selected for the KCRV value, which was determined as 2.74 µg/kg with a Standard uncertainty of 0.03 µg/kg. The 10 institutes those were included in the calculation of the consensus KCRV all agreed within their Standard uncertainties. Successful participation in CCQM-K146 demonstrates the measurement capabilities in determining mass fraction of organic compounds, with molecular mass of 100 g/mol to 500 g/mol, having low polarity pKow < -2, in mass fraction range from 0.1 µg/kg to 1000 µg/kg in a high fat, low protein, low carbohydrate food matrix.