A GC/MS method for the determination of 16 European priority polycyclic aromatic hydrocarbons in smoked meat products and edible oils

Institute for Chemistry and Physics, Federal Research Centre for Nutrition and Food, Kulmbach, Germany.
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment (Impact Factor: 1.8). 06/2008; 25(6):704-13. DOI: 10.1080/02652030701697769
Source: PubMed


A gas chromatography-mass spectrometry (GC-MS) method was developed for the analysis of 15 polycyclic aromatic hydrocarbons (PAHs) highlighted as carcinogenic by the Scientific Committee on Food (SCF) plus benzo[c]fluorine (recommended to be analysed by the Joint FAO/WHO Expert Committee on Food Additives (JECFA) in fat-containing foods such as edible oils and smoked meat products. This method includes accelerated solvent extraction (ASE) and the highly automated clean-up steps gel permeation chromatography (GPC) and solid-phase extraction (SPE). Using a VF-17ms GC column, a good separation of benzo[b]fluoranthene, benzo[j]fluoranthene and benzo[k]fluoranthene was achieved. Futhermore, the six methylchrysene isomers and the PAH compounds with a molecular weight of 302 Daltons in fat-containing foods attained a better chromatographic separation in comparison with a 5-ms column. The reliability of the analytical method for edible oils was demonstrated by the results from a proficiency test. Measurements with GC-high-resolution mass spectroscopy (HRMS) and gas chromatography-mass selective detection (GC-MSD) led to comparable results. A survey of the 16 PAHs in 22 smoked meat products showed concentrations in the range < 0.01-19 microg kg(-1). The median concentration for benzo[a]pyrene was below 0.15 microg kg(-1).

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    • "The chromatographic conditions chosen (VF-17ms) did not allow the separation of CHR and triphenylene (TP). Therefore, both CHR+TP were determined in sum (Jira et al., 2008). "
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    ABSTRACT: Benzo[a]anthracene (BaA), chrysene (CHR), cyclopenta[c,d]pyrene (CPP), 5-methylchrysene (5MC), benzo[b]fluoranthene (BbF), benzo[k]fluoranthene (BkF), benzo[j]fluGoranthene (BjF), benzo[a]pyrene (BaP), dibenzo[a,h]anthracene (DhA), indeno[1,2,3-cd]pyrene (IcP), benzo[g,h,i]perylene (BgP), dibenzo[a,l]pyrene (DlP), dibenzo[a,e]pyrene (DeP), dibenzo[a,i]pyrene (DiP) and dibenzo[a,h]pyrene (DhP), the 15 SCFPAH, assessed to be relevant as well as benzo[c]fluorene (BcL) recommended by the European Food Safety Authority (EFSA), were analysed in different types of chocolate. The sample preparation included accelerated solvent extraction (ASE), size exclusion chromatography (SEC) and solid phase chromatography using small silica gel columns. The individual PAH were separated by gas chromatography using a VF-17ms GC column and detected by high resolution mass spectrometry (HRMS). The investigation of 40 samples of various types of chocolate with different cocoa contents resulted in a median benzo[a]pyrene (BaP) content of 0.22 mu g/kg. Furthermore, the results showed a linear correlation between the content of BaP and the sum content of the 16 priority PAH. Therefore, the analysis of BaP as a leading substance seems to be suitable to estimate the PAH contamination in chocolate.
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    ABSTRACT: This paper reports a simple, fast, and inexpensive method for the determination of polycyclic aromatic hydrocarbons (PAH) in edible oils. The sample was dissolved in solvents, and a portion of the solution was loaded onto a solid phase extraction cartridge. The oil from the cartridge was washed away by isooctane/cyclohexane mixture and the absorbed PAHs were eluted with hexane/ dichloromethane mixture. GC-tandem MS was used to analyze 15 PAHs of EU priority in sesame oil and perilla oil. Analytical limits of determination (LOD) were 0.01–0.06 μg/kg, limits of quantitation (LOQ) were 0.03–0.17 μg/kg, and the recovery values ranged 55.1–105.0%. This method was validated using the certified reference material (CRM) and the error values ranged 2.06–4.30%. Twentyone commercial samples were analyzed to determine their PAHs contamination levels. The total concentration of the 15 PAHs in commercial samples ranged from not detected to 9.627 μg/kg. Only 1 sample had excessive benzo(a)pyrene content, which was more than 2.0 μg/kg.
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    ABSTRACT: For the analysis of the 16 PAH (EFSA-PAH), which are classified as priority for different food groups by the Scientific Committee on Food (SCF) and the Joint FAO/WHO Experts Committee on Food Additives (JECFA) in tea, a sensitive analytical Fast-GC/HRMS method was used. The sample preparation included accelerated solvent extraction (ASE) and the highly automated clean up steps, gel permeation chromatography and solid phase extraction. The analytical parameters, limit of detection (0.01–0.02μg/kg) and limit of quantification (0.03–0.06μg/kg), were determined. The repeatability (RSD, n=3) of different PAH in fruit tea ranged from 0.1 to 11%. It was observed that the total contents of the 16 PAH in tea samples ranged from 14 to 2,662μg/kg. The analysed tea samples showed an increasing presence of PAH in the following order: herbal and fruit tea (n=7)<black tea (n=11)<green tea (n=11)<white tea (n=3)<mate-tea (n=8). The correlation coefficient (R) between BaP and the sum of the 16 EFSA-PAH was established considering the contamination amount in all the 40 tea samples analysed.
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