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The goal of this work was the isolation of PCBs from different environmental matrices by means of solid-phase (SPE) extraction and gas chromatography/mass spectrometry (GC/MS). The analyses include the determination of PCBs in fourteen samples of transformer oils and different kinds of fodders (for poul­try, pigs, and cattle). The recovery rates for different congeners were on the level of 75-85%. The detec­tion limits of five congeners of PCBs were in the range 85 to 130 ug/kg. The RSD was on the level of 2.7 - 4.4%. The Ishikawa diagram was used for evaluation of uncertainty.
Background. Numerous studies have demonstrated acrylamide to be both neurotoxic and carcinogenic. At present it is widely recognised that acrylamide is mainly formed through the Maillard reaction from free asparagine and reducing sugars. The major sources of dietary acrylamide are potato products, processed cereals and coffee. Objective. To optimise and validate an analytical method for determining acrylamide in coffee by liquid chromatography and tandem mass spectrometry analysis (LC/MS/MS) using SPE clean-up. Material and methods. Analytical separation of acrylamide from roasted coffee was performed by liquid chromatography using a Hypercarb column followed by LC/MS/MS analysis, with 2,3,3–d3 acrylamide as an internal standard. The method was based on two purification steps: the first with hexane and Carrez solutions in order to remove of fat and to precipitate proteins, respectively; and the second with a solid-phase extraction (SPE) column which proved to be efficient in the elimination of the main chromatographic interferences. Results. Limit of quantification (LOQ) for measuring acrylamide in coffee was 50 μg/kg. The described method demonstrates satisfactory precision (RSD = 2.5%), repeatability (RSD = 9.2%) and accuracy (mean recovery – 97.4%). Conclusions. Our results confirm that LC-MS/MS with SPE clean-up is selective and suitable for determination of acrylamide in coffee. Indeed, this method meets the criteria of EU Commission Recommendations (No. 2007/331/EC and No. 2010/307/EU), on the monitoring of acrylamide levels in food.
This paper presents the biodegradation process carried out in water samples. Aliphatic hydrocarbons were degraded in the presence of the emulsifier. Non-ionic surfactant was used as the emulsifier. Two bacteria strains from the Pseudononaceae family were used in this process. We used Solid-Phase Extraction and gas chromatography for qualitative and quantitative determination of the components of the biodegradation process.
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