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

Report on the Third Inter-Laboratory Comparison Test Organised by the Community Reference Laboratory for Polycyclic Aromatic Hydrocarbons - 15+1 EU Priority PAHs in Sausage Meat and Acetonitrile

This report presents the results of the 3rd inter-laboratory comparison (ILC) of the Community Reference Laboratory for Polycyclic Aromatic Hydrocarbons (PAHs) on the determination of the 15+1 EU priority PAHs in sausage meat and acetonitrile, which was conducted along the lines of the IUPAC International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories. In agreement with the National Reference Laboratories, the test materials used in this exercise were a canned sausage meat preparation spiked with the 15+1 EU priority PAHs and a solution of the analytes in acetonitrile, respectively. The materials were prepared gravimetrically. The assigned concentration values of PAHs in sausage meat and in acetonitrile were calculated from the gravimetric preparation data. Only officially nominated National Reference Laboratories of the EU Member States and from countries covered by the Technical Assistance and Information Exchange programme of the European Commission were admitted as participants. However, from latter countries only one laboratory reported results. The participants were free to choose the method for the analysis of the materials. The performance of the participating laboratories was expressed as z-scores, which were calculated from the participants reported ¿final result¿ for the analytes' contents in the sausage meat material, based on gravimetrical preparation. The reported values of the laboratories for PAHs in acetonitrile were not rated. For the sausage meat material 88 % of the reported values were attributed with z-scores = |2|), indicating that most of the participating laboratories were performing satisfactorily with respect to internationally accepted standards. However, in some cases bias and/or a high variability were discovered, and some analytes consistently caused specific problems. It is therefore recommended to investigate this further.JRC.D.8-Food safety and qualit

Development and Optimisation of a Dopant Assisted Liquid Chromatographic-Atmospheric Pressure Photo Ionisation-Tandem Mass Spectrometric Method for the Determination of 15 + 1 EU Priority PAHs in Edible Oils

European food legislation defines a set of 16 polycyclic aromatic hydrocarbons (PAHs) as of high concern for human health. The EU set contains structurally very similar PAHs with ring numbers between 4 and 6, and so raises some separation aspects and problems, which were not experienced with traditionally analysed PAHs. Many of the currently applied gas chromatographic mass spectrometric (GC-MS) methods suffer from separation problems, while high performance liquid chromatography with fluorescence detection (HPLC-FLD) is neither capable of detecting the whole set of EU priority PAHs nor does it (compared to GC-MS) allow structural identification. In addition HPLC-FLD shows limitations with difficult matrices due to interferences. The aim of this paper is to fill this gap by describing a liquid chromatographic dopant assisted atmospheric pressure photo ionisation tandem mass spectrometric (LCDA-APPI-MS/MS) method for the determination of 15 + 1 EU priority PAHs in edible oil, which complies with the requirements set by European food legislation. Measurements were performed in positive ion mode. Anisole at a flow rate of 30 microl/min was used as dopant. Sample preparation was performed offline by donor-acceptor complex chromatography (DACC). Compared to HPLC-FLD methods the presented method enables the determination of all 15 + 1 EU priority PAHs at the low microg/kg concentration range including less fluorescence active compounds like benzo[j]fluoranthene and indeno[1,2,3-cd]pyrene. By analysing four reference materials it could be demonstrated that this method provides accurate results and is sufficiently sensitive for food control purposes. Statistically significant differences between the reference values and the measured analyte contents were not found. The method performs well also for very complex samples. Repeatability relative standard deviations (RSDr) of the determination of the target PAHs in olive oil were for most analytes below 5%. The limit of detection (LOD) of the method met the requirement set by EU legislation (0.3 microg/kg).JRC.DG.D.6-Food Safety and Qualit

Coupled Turbulent Flow Chromatography: LC-MS/MS Method for the Analysis of Pesticide Residues in Grapes, Baby Food and Wheat Flour Matrices

This paper describes an on-line sample preparation method for the simultaneous determination of 48 pesticides in grapes, baby food and wheat flour matrices. Target pesticides were selected to represent a wide variety of chemical structures and three typical matrices were selected. Turbulent flow chromatography was applied for on-line sample cleanup directly coupled to LC-MS/MS. The aim of the method was to reduce total analysis time, eliminate manual laboratory work, provide clean extracts and achieve reproducible results. Single laboratory method validation was conducted establishing limits of detection between 0.8 and 6.0 ng g(-1) for baby food, and 0.8-10.3 ng g(-1) for other matrices. Within-day precision values varied between 4 and 18 %, while between-day precisions were in the range 5-22 %. Method recovery ranged from 67 to 124 %, and method accuracy was demonstrated by analysis of external quality control samples. The method was also tested on 24 different survey samples from both bio and organic origin. The method was shown to be convenient, fast and fit for purpose in meeting regulatory requirements for pesticide residue monitoring

Report on the 5th Inter-Laboratory Comparison organised by the Community Reference Laboratory for Polycyclic Aromatic Hydrocarbons- 15 +1 EU Priority PAHs in Edible Oil and Acetonitrile

This report presents the results of the 5th inter-laboratory comparison organised by the CRL PAHs on the determination of the 16 EU priority PAHs in edible oil and acetonitrile. The test materials used in this exercise were olive oil spiked with the 16 PAHs and a solution in acetonitrile of the 16 PAHs. For the oil 83% of results were rated as satisfactory with regard to performance.JRC.DDG.D.6-Food Safety and Qualit

Report on the Inter-Laboratory Comparison Test on 15+1 EU Priority PAHs in Acetonitrile

The Institute for Reference Materials and Measurements (IRMM) of the European Commission's Joint Research Centre hosts the Community Reference Laboratory for Polycyclic Aromatic Hydrocarbons in Food (CRL-PAH). One of its core tasks is to organise inter-laboratory comparisons (ILCs) for the National Reference Laboratories (NRLs). This report presents the results of the 1st ILC of the CRL-PAH on the determination of the 15+1 EU priority PAHs in acetonitrile, which was conducted along the lines of the International Harmonized Protocol for the Proficiency Testing of Analytical Chemical Laboratories. The test material used in this exercise was a solution of the 15+1 EU priority PAHs in acetonitrile. The solution was prepared gravimetricallyJRC.D.8-Food safety and qualit

CCDC 718771: Experimental Crystal Structure Determination

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures

CCDC 718773: Experimental Crystal Structure Determination

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures

CCDC 718772: Experimental Crystal Structure Determination

An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures