Razvoj GC-FID metode za določanje frakcij ogljikovodikov iz mešanice mineralnih olj v embalaži in živilih

magistrsko delo študijskega programa II. stopnje

Kristina Preskar (Author), Mitja Kolar (Mentor), Peter Krajnc (Co-mentor), Ladislav Küčan (Co-mentor)

Abstract

V sklopu magistrskega dela je bila razvita GC–FID metoda za ločevanje in določanje aromatskih (AOMO) in nasičenih (NOMO) ogljikovodikov iz mešanice mineralnih olj v referenčnih vzorcih embalaže in živil v različnih koncentracijskih območjih (za karton v območju od 50 µg/g kartona do 3600 µg/g kartona, za riž od 4 µg/g riža do 288 µg/g riža in za jedilno (repično) olje od 30 µg/g jedilnega olja do 1709 µg/g jedilnega olja). Metoda ob predhodni pripravi vzorcev z ekstrakcijo na trdni fazi (SPE) omogoča dobro ločbo NOMO in AOMO. Za določanje teh frakcij smo uporabili plinsko kromatografijo s plamensko ionizacijskim detektorjem (GC–FID). Frakcije smo potrdili z uporabo internega standarda za skupini spojin pri enakih kromatografskih pogojih. Rezultate vsebnosti analiziranih frakcij smo statistično ovrednotili z nekaterimi validacijskimi parametri, in sicer z linearnostjo, natančnostjo kot ponovljivost in obnovljivost, točnostjo in mejo določljivosti (LOQ). Ugotovili smo, da je GC–FID metoda linearna v koncentracijskem območju od 20 µg/mL do 1440 µg/mL, s korelacijskim koeficientom (r2) nad 0,999. Potrdili smo, da je metoda ponovljiva in obnovljiva z relativnimi standardnimi odmiki (RSD) pod 25 % za frakcijo NOMO, v nekaterih primerih frakcije AOMO vrednosti odstopajo od kriterija (za cca. 25 %). LOQ za vzorec riža je bila 4 µg/g riža, za vzorec kartona 50 µg/g kartona in za vzorec jedilnega olja 30 µg/g jedilnega olja.

Keywords

ogljikovodiki mešanice mineralnih olj;embalaža;živila;ekstrakcija na trdni fazi;plinska kromatografija;plamensko ionizacijski detektor;validacija;

Data

Language:	Slovenian
Year of publishing:	2015
Typology:	2.09 - Master's Thesis
Organization:	UM FKKT - Faculty of Chemistry and Chemical Engineering
Publisher:	[K. Preskar]
UDC:	543.272.7:543.544.3(043.2)
COBISS:	19398934
Views:	1700
Downloads:	168
Average score:	0 (0 votes)
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Other data

Secondary language:	English
Secondary title:	Development of GC-FID method for the determination of hydrocarbons from mineral oil in packaging materials and foods
Secondary abstract:	The master`s thesis explores the development of GC–FID method for separation and determination of the mineral oil aromatic (AOMO) and saturated (NOMO) hydrocarbons in reference samples of packaging materials and foods in different concentration range. For a cardboard it was in the range from 50 µg/g of carboard to 3600 µg/g of cardboard, for a rice from 4 µg/g of rice to 288 µg/g of rice and for the edible (rapeseed) oil from 30 µg/g of edible oil to 1709 µg/g of edible oil. The method by preparation of samples on solid phase extraction (SPE) provides a good separation of NOMO and AOMO. For quantitative determination of these two fractions we used gas chromatography with flame ionization detector (GC–FID). The levels of each fraction were determinated at the same chromatographic conditions by using the internal standard for this group of compounds. Results of determed fractions were performed with some validation parameters such as linearity, precision as repeatability and reproducibility, accuracy and limit of quantification (LOQ). We found that is the GC–FID chromatographic system linear in the range of 20 µg/mL to 1440 µg/mL with the correlation coefficient (r2) greater than 0,999. Also we verified a method with repaeatability and reproducibility with the relative standard deviation (RSD) below 20 % for NOMO fraction but less for AOMO (cca. 25 %). The LOQ for sample of rice is 4 µg/g of rice, sample of cardboard is 50 µg/g of carboard and for sample of edible oil is 30 µg/g of edible oil.
Secondary keywords:	mineral oil hydrocarbons;packaging material;foods;solid phase extraction;gas chromatography;flame ionization detector;validation;
URN:	URN:SI:UM:
Type (COBISS):	Master's thesis/paper
Thesis comment:	Univ. v Mariboru, Fak. za kemijo in kemijsko tehnologijo
Pages:	XI, 76 str.
ID:	9078740