Certification of the Mass Fractions of Vitamins in Whole Milk Powder - Certified Reference Material ERM®-BD600

This report describes the production of the reference material ERM-BD600, a whole milk powder certified for the mass fractions of water- and fat-soluble vitamins. All the required steps during the production were conducted according to ISO Guides 34 and 35 [1,2] to ensure the high quality of the final product, including matrix material processing, homogeneity and stability studies and value assignment. The matrix material, a spray dried whole milk powder, was packed into sachets containing approximately 100 g of powder, and stored at -30 ºC. Dedicated studies confirmed the homogeneity and stability of the vitamins in the milk powder under the conditions evaluated. The characterisation of the material, organised and coordinated by IRMM, was done by an inter-laboratory comparison. The certified and indicative values were obtained as the unweighted mean of the laboratory means of the accepted sets of results for each analyte, and the expanded uncertainty associated (k = 2) includes contributions from the homogeneity, the long term stability and the characterisation of the material.JRC.D.2-Reference material

Guidance Document on the Use of Reference Materials in Genetic Testing

The aim of this guidance document is to provide a short and user-friendly support to genetic testing laboratories. It is based on internationally harmonised basic concepts and terminology for quality assurance and control (QA/QC). Relevant terms of the International Organization for Standardization (ISO) and the International Vocabulary of Metrology (VIM) are explained and references to other expert texts are provided. The document includes discussion and clarification of several often misunderstood issues. It takes into account the current scientific knowledge and the existing technological capabilities. This document may be revised and constitutes a deliverable of th NoE EuroGentest.JRC.D.2-Reference material

The Certification of the Mass Fraction of Chloramphenicol in Pork Meat - Certified Reference Material ERM®-BB130

This report describes the preparation of the pork meat matrix reference material ERM-BB130 and the certification of the content (mass fraction) of chloramphenicol. The preparation and processing of the material, homogeneity and stability studies, and the characterisation are described hereafter and the results are discussed. Uncertainties were calculated in compliance with ISO Guide 98-3, Guide to the Expression of Uncertainty in Measurement (GUM) [1] and include uncertainties due to possible heterogeneity, instability, and characterisation.JRC.DG.D.2-Reference material

The Certification of the Mass Fraction of Oxytetracycline in Partially Skimmed Milk - Certified Reference Materials ERM®-BB492 and ERM®-BB493

This report describes the preparation of two milk powder matrix reference materials (ERM-BB492 and ERM-BB493) and the certification of their content (mass fraction) of oxytetracycline. The preparation and processing of the material, homogeneity and stability studies, and the characterisation are described hereafter and the results are discussed. Uncertainties were estimated in compliance with ISO Guide 98-3, Guide to the Expression of Uncertainty in Measurement (GUM) [1]. For ERM-BB492, the uncertainty contains contributions from possible heterogeneity, instability, characterisation, and purity of the common calibrant.JRC.DG.D.2-Reference material

Determination of Short-Chain Chlorinated Paraffins by Carbon Skeleton Gas Chromatography

Short-Chain Chlorinated Paraffins (SCCPs) are highly complex technical mixtures of polychlorinated n-alkanes with a chlorination degree between 50 and 70 % by mass, and a linear carbon chain length from C10 to C13, constituted by thousands of homologues, diastereomers and enantiomers. They have been used in many different applications, such as extreme pressure additives in lubricants and cutting fluids, plasticizers in PVC, and flame retardants in paints, adhesives and sealants. SCCPs are toxic towards aquatic organisms, bioaccumulative and persistent, and therefore the concern about this class of pollutants has increased in the last few years. In 2000 the European Union has included SCCPs in the list of priority substances in the field of water policy, amending the Water Framework Directive (WFD) 2000/60/EC. The implementation of the directive requires that laboratories should be able to measure such substances reliably at the level of the environmental quality standard (EQS). Unfortunately, this is not the case for SCCPs. The analytical tools currently available for the analysis of this class of compounds are scarce and no methodology has been fully validated. This is due to the complexity of their mixtures, and the lack of pure solutions for calibrations as well as matrix-matched reference materials. No routine method for monitoring purposes exists and a poor comparability of results was demonstrated. At present determination of SCCPs is mostly performed by mass spectrometry (MS) in the Electron Capture Negative Ionisation (ECNI) mode. The quantification relies on the monitoring of [M-Cl]- ions of specific mass to charge (m/z) ratio for each SCCP group according to the method developed by Tomy et al. This approach is prone to interferences from other chlorinated compounds and from medium chain chlorinated paraffins, therefore a thorough clean-up of the sample and a careful selection of the ions to be detected are necessary. The method is also affected by a strong dependence on the degree of chlorination of the standard used for calibration. Errors of up to 1100 % have been reported when the calibrant does not match the chlorination degree of the sample. An alternative approach for SCCPs determination is the carbon skeleton gas chromatography (GC)-MS in which chlorinated paraffins are catalytic hydrodechlorinated to the corresponding n-alkanes (see Figure 1). Information on the chlorination degree is lost, but accurate quantification is possible. In this paper the two approaches are compared, and some preliminary results in the determination of SCCPs in water samples with the carbon skeleton method are presented.JRC.DG.D.2-Reference material

The Certification of the Mass Fractions of Stilbenes in Bovine Urine - Certified Reference Materials ERM®-BB386 and ERM®-BB389

This report describes the preparation of the pork meat matrix reference materials ERM BB386 and ERM-BB389 and the certification of the content (mass fraction) of three stilbenes. The preparation and processing of the material, homogeneity and stability studies, and the characterisation are described hereafter and the results are discussed. Uncertainties were calculated in compliance with the ISO/IEC Guide 98-3 Guide to the Expression of Uncertainty in Measurement (GUM) [1] and include uncertainties due to possible heterogeneity, instability, and characterisation.JRC.D.2-Standards for Innovation and sustainable Developmen

Training manual on GMO quantification: Proper calibration and estimation of measurement uncertainty

The content of this manual is based on the training course that was organised on the premises of the European Commission, Joint Research Centre, Institute for Reference Materials and Measurements (Geel, BE) at the end of 2013. The training manual complements the training course that was intended to improve the quality of measurement results obtained when quantifying genetically modified organisms (GMO) in food and feed. Both, the training course and this manual, were developed in line with the current EU GMO legislation. The manual is addressed to laboratory managers and practitioners in analytical laboratories who perform GM quantification measurements and use reference materials for calibration, quality control and method validation including in-house verification. It is also intended for analysts who need to assess measurement uncertainties as required by (EC) No 1829/2003, (EC) No 619/2011 and ISO/IEC 17025:2005. This training document has been written by JRC-IRMM upon request of the European Union Reference Laboratory for Genetically Modified Food and Feed (EURL-GMFF) to further improve the reporting of National Reference Laboratories (NRLs) nominated under Regulation (EC) No 882/2004 and official GMO control laboratories within the EU. This manual is organised in four chapters covering the proper calibration of PCR methods, the estimation of measurement uncertainty, the establishment of metrological traceability of a measurement result and the way to prove the trueness of measurement results. The training manual is a didactic support of a previous guidance document that outlines issues related to the estimation of measurement uncertainty (MU) in the GMO sector. The training manual is also in line with the European technical guidance document for the flexible scope accreditation of laboratories quantifying GMOs, that is intended for laboratories that are acquiring or are holding a flexible scope of accreditation according to ISO/IEC 17025.JRC.D.2-Standards for Innovation and sustainable Developmen

Biomonitoring of antimony in environmental matrices from terrestrial and limnic ecosystems

Elder and poplar leaves from various sampling sites were studied with respect to their antimony content. Moreover, a retrospective determination of Sb was performed in representative limnic and terrestrial samples of the Federal Environmental Specimen Bank of Germany which have been collected over 14 years. The analytical procedure is based on an open vessel acid digestion of freeze-dried biological samples and the subsequent quantification of Sb in the digests by flow injection hydride generation atomic absorption spectrometry. Strict quality control schemes were applied to the entire procedure to guarantee accurate and precise results. No long-term changes of the Sb concentrations were found in spruce shoots or poplar leaves from different sampling sites. However, spruce shoots from a semi-natural region showed concentrations of Sb (~22 ng g−1; range: 17-29 ng g−1) that were approximately four times lower than in corresponding samples from an urban-industrialized area. The analysis of virgin and washed elder leaves revealed that approximately 20-30% of the Sb is present on the leaf surface. Sb levels in elder leaves ranged from 5.2±0.3 ng g−1 in samples from Argentina to 589±30 ng g−1 in leaves collected directly beside a motorway in Germany. Similarly, poplar leaves from Argentina and Chile showed about 4 ng Sb g−1, whereas 150 ng Sb g−1 was found in poplar leaves from Germany. The lowest concentrations of Sb were determined in digests of pigeon eggs (~2 ng g−1), bream liver (~4 ng g−1) and deer liver (~6 ng g−1). A similar pattern of Sb concentrations in spruce shoots, leaves or liver samples from an industrialized area and an agrarian ecosystem in Germany was established. Concentrations of Sb in elder leaves were closely associated with car traffic, giving maximum concentrations of 589 ng g−1 directly beside a motorway, 207 ng g−1 50 m from the motorway and 153 ng g−1 in a close residential area. The concentrations of Sb in many biological samples are i