Title: 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
Authors: HOLLOSI LaszloWENZL Thomas
Citation: JOURNAL OF CHROMATOGRAPHY A vol. 1218 no. 1 p. 23-31
Publication Year: 2011
JRC N°: JRC57648
ISSN: 0021-9673
URI: http://publications.jrc.ec.europa.eu/repository/handle/JRC57648
DOI: 10.1016/j.chroma.2010.10.015
Type: Articles in periodicals and books
Abstract: 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 Directorate:Health, Consumers and Reference Materials

Files in This Item:
There are no files associated with this item.

Items in repository are protected by copyright, with all rights reserved, unless otherwise indicated.