Gas chromatography-mass spectrometry (GC-MS) method for the determination of 16 European priority polycyclic aromatic hydrocarbons in smoked meat products and edible oils.
ABSTRACT 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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ABSTRACT: Hundreds of millions of people worldwide have tattoos, which predominantly contain black inks consisting of soot products like Carbon Black or polycyclic aromatic hydrocarbons (PAH). We recently found up to 200 μg/g of PAH in commercial black inks. After skin tattooing, a substantial part of the ink and PAH should be transported to other anatomical sites like the regional lymph nodes. To allow a first estimation of health risk, we aimed to extract and quantify the amount of PAH in black tattooed skin and the regional lymph nodes of pre-existing tattoos. Firstly, we established an extraction method by using HPLC - DAD technology that enables the quantification of PAH concentrations in human tissue. After that, 16 specimens of human tattooed skin and corresponding regional lymph nodes were included in the study. All skin specimen and lymph nodes appeared deep black. The specimens were digested and tested for 20 different PAH at the same time.PAH were found in twelve of the 16 tattooed skin specimens and in eleven regional lymph nodes. The PAH concentration ranged from 0.1-0.6 μg/cm2 in the tattooed skin and 0.1-11.8 μg/g in the lymph nodes. Two major conclusions can be drawn from the present results. Firstly, PAH in black inks stay partially in skin or can be found in the regional lymph nodes. Secondly, the major part of tattooed PAH had disappeared from skin or might be found in other organs than skin and lymph nodes. Thus, beside inhalation and ingestion, tattooing has proven to be an additional, direct and effective route of PAH uptake into the human body.PLoS ONE 03/2014; 9(3):e92787. DOI:10.1371/journal.pone.0092787 · 3.53 Impact Factor
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ABSTRACT: For the analysis of 15 + 1 EU priority PAH in tea and herbal infusions, an online-SPE-LVI-GC-MS method was developed. This method includes sample extraction of the tea and herbal infusions with saponification followed by an automated SPE clean-up step. For brews a liquid-liquid extraction with cyclohexane was performed before an automated SPE clean-up. Gas chromatographic separation was done using an Agilent J&W Select PAH (15 m × 0.15 mm × 0.10 µm) column which allows the separation of the three benzofluoranthenes as well as triphenylene from chrysene. Method performance criteria such as method linearity, LOQ and repeatability were determined and demonstrated the method being fit-for-purpose. The method was used to analyse 15 + 1 EU priority PAH in 91 tea and herbal infusion samples. The levels of PAHs ranged from below 0.5 (LOQ) to 460 µg kg(-1) with a median amount of 4.7 µg kg(-1) and a mean amount of 39 µg kg(-1) for BaP, and from below 1.0 (LOQ) to 2700 µg kg(-1) with a median value of 39 µg kg(-1) and a mean of 250 µg kg(-1) for total PAH which were in good agreement with other studies reported in literature. For the brews prepared under normal house preparation (20 g material in 2 l boiling tap water for 10 min) no total 15 + 1 PAH could be detected above the LOQ. With an extended brewing time of 30 min a transfer rate between 0.25% and 0.52% could be determined which results in no exceeding of the maximum limits given by the EU directive for drinking water (EU Council directive 98/83/EC).Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment 09/2014; 31(10). DOI:10.1080/19440049.2014.952785
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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.Food science and biotechnology 02/2013; 22(1). DOI:10.1007/s10068-013-0073-1 · 0.66 Impact Factor