Metrological Assurance of Dioxin Measurements. A Certified Reference Material for Measuring the Dioxin Mass Fraction in Animal Fat

Author(s):  
Alexandra G. Budko ◽  
Alena Y. Mikheeva ◽  
Anatoliy I. Krylov
2019 ◽  
Vol 14 (3-4) ◽  
pp. 17-32 ◽  
Author(s):  
A. G. Budko ◽  
A. Y. Mikheeva ◽  
A. I. Krylov

The paper presents information on the development of a new certified reference material (CRM) for mass fraction of dioxins in animal fat, with established metrological traceability. A procedure for preparing and certifying CRM material is given. The GC–LRMS method with isotopic dilution was used as an analytical method for establishing certified characteristics. The uncertainties due to inhomogeneity and instability of the CRM material were estimated in order to account for their contribution to the uncertainty of certified values. In addition, the results of interlaboratory comparisons (ILC) for an experimental batch of the developed CRM are presented. Measurement results provided by ILC participants are shown to be in good agreement with the certified characteristics of the CRM. The certified values of dioxin mass fractions (PCDF group) in the CRM material are established to vary from 1 to 1000 ng / kg, with the relative expanded uncertainty ranging from 10 to 20 %.


2020 ◽  
Vol 412 (19) ◽  
pp. 4483-4493
Author(s):  
Akane Yamakawa ◽  
Sylvain Bérail ◽  
David Amouroux ◽  
Emmanuel Tessier ◽  
Julien Barre ◽  
...  

Minerals ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 92
Author(s):  
Said Kounbach ◽  
Mokhtar Ben Embarek ◽  
Abdeljalil Chemaa ◽  
Rachid Boulif ◽  
Rachid Benhida ◽  
...  

Fluosilicic acid is a by-product of the chemical phosphate industry, mainly during the manufacture of phosphoric acid and triple super phosphate (TSP). To ensure the accurate measurement of the H2SiF6 mass fraction in this by-product, method validation is required, which needs a certified reference material (CRM) with its traceability to the International System of Units (SI). This work describes the development of a certified reference material of fluosilicic acid, which is commercially unavailable. Details of all steps, such as sample preparation, homogeneity and stability studies, value assignment, establishment of metrological traceability, and uncertainty estimation of the certified reference material, are fully described. The H2SiF6 mass fraction in the CRM was quantified by two analytical methods, i.e., UV-VIS as a primary method of analysis and flame mode atomic absorption spectroscopy (AAS) as a second method. It is worth noting that the results obtained from each method were in good agreement. The CRM certified value and corresponding expanded uncertainty, obtained from the combined standard uncertainty multiplied by the coverage factor (k = 2), for a confidence interval of 95%, was (91.5 ± 11.7) g·kg−1. The shelf life of the developed CRM is determined to be 1 year, provided that storage conditions are ensured. The developed CRM can be applied to validate analytical methods, improve the accuracy of measurement data as well as to establish the meteorological traceability of analytical results.


Author(s):  
Juliane Riedel ◽  
Sebastian Recknagel ◽  
Diana Sassenroth ◽  
Tatjana Mauch ◽  
Sabine Buttler ◽  
...  

AbstractZearalenone (ZEN), an estrogenic mycotoxin produced by several species of Fusarium fungi, is a common contaminant of cereal-based food worldwide. Due to frequent occurrences associated with high levels of ZEN, maize oil is a particular source of exposure. Although a European maximum level for ZEN in maize oil exists according to Commission Regulation (EC) No. 1126/2007 along with a newly developed international standard method for analysis, certified reference materials (CRM) are still not available. To overcome this lack, the first CRM for the determination of ZEN in contaminated maize germ oil (ERM®-BC715) was developed in the frame of a European Reference Materials (ERM®) project according to the requirements of ISO Guide 35. The whole process of CRM development including preparation, homogeneity and stability studies, and value assignment is presented. The assignment of the certified mass fraction was based upon an in-house study using high-performance liquid chromatography isotope dilution tandem mass spectrometry. Simultaneously, to support the in-house certification study, an interlaboratory comparison study was conducted with 13 expert laboratories using different analytical methods. The certified mass fraction and expanded uncertainty (k = 2) of ERM®-BC715 (362 ± 22) μg kg−1 ZEN are traceable to the SI. This reference material is intended for analytical quality control and contributes to the improvement of consumer protection and food safety. Graphical abstract


2011 ◽  
Vol 400 (3) ◽  
pp. 821-833 ◽  
Author(s):  
Pearse McCarron ◽  
Håkan Emteborg ◽  
Cíara Nulty ◽  
Thomas Rundberget ◽  
Jared I. Loader ◽  
...  

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