Razvoj i validacija kromatografske metode za određivanje nitrozo-spojeva

master's thesis

• Title (english): Development and validation of a chromatographic method for the determination of nitroso compounds
• Author: Valentino Golub
• Mentor: Sandra Babić (mentor)
• Committee member: Sandra Babić (predsjednik povjerenstva)
• Committee member: Dragana Mutavdžić Pavlović (član povjerenstva)
• Committee member: Krešimir Košutić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2022-09-09, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

U ovom radu razvijena je SPE-HPLC-DAD metoda za određivanje pet N-nitrozamina u vodi: N-nitrozodietilamina (NDEA), N-nitrozodipropilamina (NDPA), N-nitrozodibutilamina (NDBA), N-nitrozopirolidina (NPYR) i N-nitrozomorfolina (NMOR). Za pripremu uzorka vode primijenjena je ekstrakcija čvrstom fazom (SPE) uz korištenje sorbensa od kokosovog ugljena. Uspješna kromatografska separacija svih pet analita postignuta je na Kinetex 5 μm C18 koloni 100 Å, 150 x 4,6 mm, uz pokretnu fazu sastavljenu od MilliQ vode i acetonitrila te gradijentno eluiranje pri protoku 0,5 mL min^-1. Razvijena SPE-HPLC-DAD metoda je validirana pri čemu su ispitane sljedeće izvedbene karakteristike: selektivnost, linearnost, granice detekcije i kvantifikacije te točnost kroz istinitost i preciznost. Postignuta je dobra linearnost uz koeficijente korelacije veće od 0,99, dobra preciznost uz RSD < 10 % te dobro iskorištenje unutar raspona 70 – 120 % za sve ispitivane analite. Metoda je uspješno primijenjena u analizi uzoraka tijekom reverzno osmotske membranske separacije: ulazne otopine, permeata i retentata.

Abstract (english)

In this work, a SPE-HPLC-DAD method was developed for the determination of five N-nitrosamines in water: N-nitrosodiethylamine (NDEA), N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA), N-nitrosopyrrolidine (NPYR) and N-nitrosomorpholine (NMOR). For the preparation of the water sample, solid phase extraction (SPE) was applied with the use of coconut charcoal sorbent. Successful chromatographic separation of all five analytes was achieved on a Kinetex 5 μm C18 column 100 Å, 150 x 4.6 mm, with a mobile phase composed of MilliQ water and acetonitrile and gradient elution at a flow rate of 0.5 mL min^-1. The developed SPE-HPLC-DAD method was validated by testing the following performance characteristics: selectivity, linearity, limits of detection and quantification, and accuracy through trueness and precision. Good linearity with correlation coefficients higher then 0.99, good precision with RSD < 10% and good extraction recovery within the range of 70-120% for all analyzed analytes was achieved. The method was successfully applied in the analysis of samples during reverse osmosis membrane separation: feed solution and permeate and retentate.

• Keywords: N-nitrozamini; voda; SPE-HPLC-DAD; validacija metode
• Keywords (english): N-nitrozamines; water; SPE-HPLC-DAD; method validation
• Language: croatian
• URN:NBN: urn:nbn:hr:149:520708
• Study programme: Title: Applied Chemistry - Graduate study; specializations in: Environmental chemistry and green technologies, Advanced materials and technologies, Applied organic chemistry; Course: Applied organic chemistry; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra primijenjene kemije (magistar/magistra primijenjene kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2023-09-09
• Created on: 2023-03-10 16:01:25