Proficiency Test on the Determination of Acrylamide in Potato Crisps

The Institute for Reference Materials and Measurements (IRMM) of the European Commission¿s Joint Research Centre (JRC) was requested by the Directorate General Health and Consumer Protection (DG SANCO) to organise a proficiency test on the determination of acrylamide in potato products in 2007. The aim of this test was to support the implementation of the acrylamide monitoring Recommendation 2007/331/EC. The organisation of the study as well as the evaluation of the results was done in accordance with ¿The International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories¿. The potato crisps used for the preparation of the test material was produced in a pilot plant of the German Federal Research Centre for Nutrition and Food (Detmold, Germany). The study was free of charge for the participants. Altogether forty two laboratories from 16 EU Member States subscribed for participation in the study. The participants were asked to determine the acrylamide content in the test sample by application of their usual in-house analysis methods. The laboratories were requested to report the results via a web-interface into a secured databank. In total, 36 result data sets were reported to the organisers of the study. Details regarding the applied analytical methods were requested from the participants. Thirty one participants filled in and returned the questionnaire with the method details back to the organisers. An assigned value for the acrylamide content of the test material was established by an isotope dilution HPLC-MS/MS method. The target standard deviation was calculated according to a proposal of Thompson, which applies a concentration dependent modification of the Horwitz equation. The performance of laboratories was expressed by the z-score. They are considered satisfactory if the values of |z| = 2. Twelve laboratories of 36 (33.3%) reported results |z| >2. The percentage of successful laboratories is lower in comparison to previous proficiency tests organised by IRMM as well as to the last FAPAS® round. Reasons for this might be a more complex food matrix and/or the application of improper methods. However, the study showed the importance of continuous participation in proficiency testing schemes in order to achieve comparability of results.JRC.D.8-Food safety and qualit

Report on the 8th inter-laboratory comparison organised by the European Union Reference Laboratory for Polycyclic Aromatic Hydrocarbons : Four marker PAHs in a dry extract of St John's wort

The proficiency test here reported concerned the determination of the contents of four marker polycyclic aromatic hydrocarbons (PAHs), and of their sum in an food supplements test sample. The set of marker PAHs consists of benz[a]anthacene, benzo[a]pyrene, benzo[b]fluoranthene, and chrysene. Participants to these PT were National Reference Laboratories for PAHs (NRLs-PAHs) and EU official food control laboratories. The number of participants was in total 48. The PT was organised according ISO Standard 17043:2010. The test material used was a commercial dry extract of St. John's wort. Participants also received a solution of the same PAHs either in acetonitrile or in toluene for checking their instrument calibration. The results from participants were rated with z-scores and zeta-scores. About 68 % of the reported results were attributed with z-scores with an absolute value of below two, which is the threshold for satisfactory performance.JRC.D.5-Standards for Food Bioscienc

A Simple Method to Determine Critical Coagulation Concentration from Electrophoretic Mobility

Critical coagulation concentration (CCC) is a key parameter of particle dispersions, since it provides the threshold limit of electrolyte concentrations, above which the dispersions are destabilized due to rapid particle aggregation. A computational method is proposed to predict CCC values using solely electrophoretic mobility data without the need to measure aggregation rates of the particles. The model relies on the DLVO theory; contributions from repulsive double-layer forces and attractive van der Waals forces are included. Comparison between the calculated and previously reported experimental CCC data for the same particles shows that the method performs well in the presence of mono and multivalent electrolytes provided DLVO interparticle forces are dominant. The method is validated for particles of various compositions, shapes, and sizes

Validation of an Analytical Method to Determine the Content of Acrylamide in Roasted Coffee

An inter-laboratory comparison study was carried out to evaluate the effectiveness of a method that was standardised for the determination of acrylamide in bakery and potato products for the determination of acrylamide in roasted coffee. The intention was to extend the scope of the standardised method to roasted coffee. Therefore only slight modifications of the standardised method were tolerated. The method is based on aqueous extraction of the roasted coffee matrix and solid phase extraction (SPE) clean-up followed by isotope dilution high performance liquid chromatography with tandem mass spectrometric detection (LC-MS/MS). The test portion of the sample was spiked with isotope labelled acrylamide and extracted on a mechanical shaker with n-hexane and water for one hour. The sample extract was centrifuged, the organic phase was discarded, and a portion of the aqueous extract was further cleaned-up by solid phase extraction on Isolute Multimode followed by Isolute ENV+ columns. The acrylamide-containing fraction eluted from the second SPE column was evaporated to about 500 µL and analysed by reverse-phase high performance liquid chromatography (HPLC) with tandem mass spectrometric detection. Three coffee samples and one aqueous acrylamide standard solution (quality control sample) were sent to 11 laboratories from 8 EU Member States. All samples were sent as blinded duplicates. Based on the reported results the relative standard deviations for reproducibility (RSDR) were 11.5 % at an acrylamide level of 160 µg/kg, 10.1 % at a level of 263 µg/kg, and 9.6 % at a level of 585 µg/kg. The values for RSDr in those materials ranged from 1 % to 3.5 %.JRC.D.8-Food safety and qualit

Report on the 7th Inter-Laboratory Comparison Organised by the European Union Reference Laboratory for Polycyclic Aromatic Hydrocarbons - 15 + 1 EU Priority PAHs in Spiked Olive Oil and Solvent Solution

The European Union Reference Laboratory for PAHs (EU-RL-PAHs), operated by the Institute for Reference Materials and Measurements (IRMM) of the Joint Research Centre (JRC), organises yearly one or more proficiency tests (PTs) within the scope of the Regulation (EC) 882/2004. The proficiency test here reported concerned the determination of the 15+1 EU priority polycyclic aromatic hydrocarbons (PAHs) in an olive oil test sample. Participants to these PT were National Reference Laboratories for PAHs (NRLs-PAHs) and EU official food control laboratories. The number of participants was 54. The PT was organised along the lines of the IUPAC Harmonised Protocol for the Proficiency Testing of Analytical Chemistry Laboratories. The test material used was olive oil spiked with a 15 + 1 EU priority PAHs and a solution of the target analytes in depending of the preference of the participants acetonitrile or toluene. The results from participants were rated with z-scores and zeta-scores. About 90 % of the reported results were attributed with z-scores with an absolute value of below two, which is the threshold for satisfactory performance.JRC.DG.D.6-Food Safety and Qualit

Report on the 4th Inter-laboratory Comparison Organised by the Community Reference Laboratory for Polycyclic Aromatic Hydrocarbons - 15 + 1 EU Priority PAHs in Fish and Acetonitrile

This report represents the results of the 4th inter-laboratory comparison organised by the CRL PAHs on the determination of the 16 EU priority PAHs in fish and acetonitrile. The test materials used in this exercise were raw, frozen fish spiked with the 16 PAHs, a cooked fish spiked with an extract of contaminated smoke flavourings and a solution in acetonitrile of the 16 PAHs. For the frozen fish 94% of results were rated as satisfactory with regard to performance. For the smoked fish 89% of results were rated satisfactory.JRC.DDG.D.6-Food Safety and Qualit

Design and baseline characteristics of the finerenone in reducing cardiovascular mortality and morbidity in diabetic kidney disease trial

Background: Among people with diabetes, those with kidney disease have exceptionally high rates of cardiovascular (CV) morbidity and mortality and progression of their underlying kidney disease. Finerenone is a novel, nonsteroidal, selective mineralocorticoid receptor antagonist that has shown to reduce albuminuria in type 2 diabetes (T2D) patients with chronic kidney disease (CKD) while revealing only a low risk of hyperkalemia. However, the effect of finerenone on CV and renal outcomes has not yet been investigated in long-term trials. Patients and Methods: The Finerenone in Reducing CV Mortality and Morbidity in Diabetic Kidney Disease (FIGARO-DKD) trial aims to assess the efficacy and safety of finerenone compared to placebo at reducing clinically important CV and renal outcomes in T2D patients with CKD. FIGARO-DKD is a randomized, double-blind, placebo-controlled, parallel-group, event-driven trial running in 47 countries with an expected duration of approximately 6 years. FIGARO-DKD randomized 7,437 patients with an estimated glomerular filtration rate >= 25 mL/min/1.73 m(2) and albuminuria (urinary albumin-to-creatinine ratio >= 30 to <= 5,000 mg/g). The study has at least 90% power to detect a 20% reduction in the risk of the primary outcome (overall two-sided significance level alpha = 0.05), the composite of time to first occurrence of CV death, nonfatal myocardial infarction, nonfatal stroke, or hospitalization for heart failure. Conclusions: FIGARO-DKD will determine whether an optimally treated cohort of T2D patients with CKD at high risk of CV and renal events will experience cardiorenal benefits with the addition of finerenone to their treatment regimen. Trial Registration: EudraCT number: 2015-000950-39; ClinicalTrials.gov identifier: NCT02545049