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Browsing by Subject "GC-MS"

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  • Isotupa, Minna (2010)
    3-Chloro-1,2-propanediol (3-MCPD) and its esterified forms are food-borne contaminants. The chemical properties of fatty acid esters of 3-MCPD and their formation in foodstuffs as well as the analytical methods used to detect them were reviewed. The aim of the experimental work was to compare the analytical methods used to detect 3- MCPD esters and to obtain a method for detection of 3-MCPD fatty acid esters in Finnish Food Safety Authority (EVIRA). Synthesised 3-MCPD palmitate esters and palm oil samples were used to detect differences between the methods. Decomposition of 3-MCPD during hydrolysis with sodium methoxide was studied as well as the formation of excess 3- MCPD in palm oil samples during acid hydrolysis. 3-MCPD fatty acid esters were determined as free 3-MCPD by GC-MS after hydrolysis and derivatisation with phenylboronic acid. Free 3-MCPD was cleaved from 3-MCPD esters using acidic hydrolysis with sulphuric acid and methanol or transesterification with sodium methoxide. The amount of 3-MCPD obtained after the hydrolysis of synthesised 3-MCPD esters with sodium methoxide was only 45 % of that obtained after acid hydrolysis. There was a statistical difference between the means at a 95 % level of significance. The formation of excess 3-MCPD during acid hydrolysis was not proven from the results obtained from the palm oil samples. Results showed the opposite, as the amount of 3-MCPD obtained was larger after hydrolysis with sodium methoxide. The precision of the results was poor possibly due to a large systematic error and should be renewed in the future. The results showed there is a significant difference between the two methods of hydrolysis and that the choice between the methods can influence the recovery of the 3-MCPD esters.
  • Pynnönen, Henna (2009)
    Methylation analysis by Ciucanu and Kerek (1984) and Hakomori (1964) and the meaning of circumstances in the reaction, reaction parameters and structure of the sample were reviewed in this study. The experimental work consisted of methylation analysis of glucose, cellobiose, isomaltose, pullulan, commercial dextran and dextrans produced by lactic acid bacteria Weissella confusa and Leuconostoc citreum. The success of the methylation was controlled using the IR-method. Methylated samples were treated by methanolysis and acid hydrolysis. The structure analyses were carried out with GC-MSspectra. Two different columns: DB-1 and HP-5 were compared in the GC-analysis. Two hours methylation in the ultrasonic bath gave good methylation results. It was easy to control the methylation by IR-method. OH-peak (3400 cm-1) was absent and CH3- peaks (2900 and 2800 cm-1) were high after successful methylation. IR-spectroscopy is a valuable tool to check if methylation has been successful. Samples could be remethylated before hydrolysis and derivation if necessary. After methanolysis there were ?- and ?-pyranose forms from each methylated monosaccharides. Due to reduction after the acid hydrolysis method, there was only one methylated form from each product. The structures of glucose, cellobiose, isomaltose and pullulan were solved by both hydrolysis methods. Recovery of these samples was good but the deviation was large. The structure of commercial dextran and dextran produced by W. confusa were solved by methanolysis method and partly by acid hydrolysis method. Recovery of these samples was poor. The methylation succeeded only in one of the dextran samples produced by L. citreum. The methylation analysis of dextrans could be developed in the future by increasing the temperature and the time of mixing and by adding some glycerol.
  • Kajaste, Riina (2018)
    The aim of this study was to determine the chemical hazards associated with the packaging materials of liquid packaging board with polyethylene coating on both sides, and if these chemical hazards would transfer to the liquid packaging board and to milk packaged in it. Consumers’ exposure to chemical hazards resulting from the packaging materials of the liquid packaging board used in the packaging of milk was assessed. Additionally, the process of safety assessment of new packaging materials of liquid packaging board was developed and described. A multinational manufacturer of food contact materials bears a great responsibility for the consumer safety and conformance of its products which is why conducting this study was important. A core made of recycled fibre and a tape used in the packaging of liquid packaging board were assessed for their chemical risk in this study. The core consists of adhesives and core board made of recycled fibre. Adhesive tapes consist of backing material and adhesive. Sometimes a primer is used between the backing material and adhesive. The chemical composition and potential sources of contamination were discussed in the literary review. Non-Intentionally Added Substances (NIAS) and substances known to cause alterations in the sensory properties of liquid packaging board and food in adhesive tapes and core board were analysed. Additionally, non-targeted screening methods were employed to detect unpredicted NIAS in the packaging materials, liquid packaging board and a food simulant for milk. The concentrations of NIAS were compared with specific migration limits in the European Commission Regulation (EU) 10/2011 on plastic materials and articles intended to come into contact with food. They were also compared with the values of acceptable and tolerable daily intakes if provided by the European Food Safety Authority (EFSA). The analytical methods that were used for qualitative and quantitative analyses were GC-MS and GC-FID. Predicted and unpredicted NIAS were detected from the packaging materials using the chosen methods. Some of the substances were found to transfer to liquid packaging board and to the food simulant. The migration to the food simulant was not be analysed for some of the NIAS. Additional information on the transfer of these substances to food is still needed. Substances for which adequate toxicological information was available did not pose a threat to consumer safety based on the exposure assessment. Furthermore, a process for the risk assessment of new packaging materials was successfully developed.