Stanovení netěkavých N-nitrosaminů ve sladu
Determination of non-volatile N-nitrosamines in malt
diploma thesis (DEFENDED)

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Permanent link
http://hdl.handle.net/20.500.11956/82835Collections
- Kvalifikační práce [15772]
Author
Advisor
Referee
Čejka, Pavel
Faculty / Institute
Faculty of Science
Discipline
Analytical Chemistry
Department
Department of Analytical Chemistry
Date of defense
1. 6. 2016
Publisher
Univerzita Karlova, Přírodovědecká fakultaLanguage
Czech
Grade
Very good
Keywords (Czech)
Netěkavé N-nitrosamíny, N-nitrosoprolin, N-nitrososarkosin, N-nitrosopipekolová kyselina, slad, plynová chromatografie, chemiluminiscenční detektor
Keywords (English)
Non-volatile N-nitrosamines, N-nitrosoproline, N-nitrososarcosine, N-nitrosopipecolic acid, malt, gas chromatography, chemiluminiscence detector
V rámci diplomovej práce bola vyvinutá a optimalizovaná metóda stanovenia N-nitrozoprolínu a N- nitrozosarkosínu v slade plynovou chromatografiou s chemiluminiscenčným detektorom. Optimalizácia extrakčnej metódy bola uskutočnená pomocou metódy odezvových plôch. Na kvantifikáciu bola použitá metóda interného štandardu (N-nitrozopipekolová kyselina), v rámci ktorej bolo potrebné overiť vplyv matricových efektov. Tie boli potvrdené v mníchovskom a plzeňskom slade, preto bolo pre kvantifikáciu nutné zostrojiť matricovú kalibračnú krivku. Vyvinutá metóda bola aplikovaná na pšeničný, mnichovský a plzeňský slad. N-nitrozoprolín bol detekovaný len v mníchovských sladoch a v ostatných prípadoch bol pod limotom detekcie (LOD=4,0 µg/kg). N-nitrososarkosín bol vo všetkých prípadoch pod limitom detekcie (LOD=3,7 µg/kg). Matricová kalibračná krivka bola zostrojená pre experimentálny mníchovský slad, kde bola koncentrácia NPRO 13,2 ± 2,9 µg/kg. Powered by TCPDF (www.tcpdf.org)
The aim of diploma thesis has been development and optimization of method determination of N- nitrososarcosine and N-nitrosoproline in malt by gas chromatography with chemiluminiscence detector. Optimization of extraction method has been performed by response surface method. Quantification has been performed by internal standard method (N-nitrosopipecolic acid, in which matrix effects has been studied. These has been verified in münchen and pilsen malt, therefore matrix-matched calibration has been constructed. The developed method has been aplicated on wheat, münchen and pilsen malt. N- nitrosoproline was detected only in münchen malt and in other cases has been under limit of detection (LOD=4,0 µg/kg). N-nitrososarcosine was in all cases under limit of detection (LOD=3,7 µg/kg). The matrix-matched calibration has been constructed for experimental münchen malt with N-nitrosoproline concentration at 13,2 ± 2,9 µg/kg. Powered by TCPDF (www.tcpdf.org)