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Chromatographic determination of amines in food samples

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Title: Chromatographic determination of amines in food samples
Author(s): Jubele, Anna
Contributor: University of Helsinki, Faculty of Science, Department of Chemistry
Discipline: Analytical Chemistry
Language: English
Acceptance year: 2018
In the first part of this thesis literature about the determination amines in food samples of the past decade (2007 – 2017) has been reviewed. The sample preparation methods and chromatographic determination methods have been reviewed. The review is focused on biogenic amines (BA) since BAs are the most relevant in food samples. Monitoring the concentration levels of BAs in foods is important because elevated levels of amine concentrations in food products can indicate spoilage which can lead to food poisoning. Food samples are complex matrices therefore sample preparation is required prior to analysis. Amine extraction methods are reviewed in more detail, including conventional solid-liquid extraction (SLE) and solid phase extraction (SPE), and novel and miniaturized methods: solid phase micro extraction (SPME), liquid phase micro extraction (LPME) and dispersive liquid-liquid micro extraction (DLLME). The derivatization methods of Bas have also been reviewed including derivatization with o - phthaldialdehyde (OPA), dansyl chloride, benzoyl chloride and diethyl ethoxymethylenemalonate (DEEMM). Chromatographic methods are well researched tools in determination of amines in food samples. In the past decade only few application were found of thin layer chromatography (TLC). The gas chromatography (GC) has been used more often, especially in the analyses of beverages. However, the high performance liquid chromatography (HPLC) is the main method of choice in determination of amines in food samples as demonstrated by the large numbers of research articles. Recently also the ultra-high performance liquid chromatography (UHPLC) has been gaining popularity. In this master’s thesis experimental part several sets of experiments were performed. Adsorbing materials were synthesized using suspension polymerization and silica gel functionalization. Compositions of materials were estimated by FTIR. The materials were characterized in terms of their suitability for amine adsorption. Ion exchange capacity was determined by titration. Static and dynamic binding capacity was determined by HPLC-UV. Derivatization studies of atmospheric amines by 9-Fluorenylmethoxycarbonyl chloride (Fmoc-Cl) were carried out by HPLC-UV. Potential imine formation was investigated by HPLC-UV. The most promising adsorbing material was a hydrolyzed copolymer of divinylbenzene and methacrylic anhydride (DVB-(MAA)2O). Its ion exchange capacity was 4.8 meq/g, static binding capacity was 0.95 mmol/g of tertiary amine and dynamic binding capacity was 2.0 mmol/g for primary amine and 0.8 mmol/g for tertiary amine.

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