Validacija HPLC-DAD metode za određivanje onečišćivala u modelnim i realnim uzorcima

undergraduate thesis

• Title (english): Validation of the HPLC-DAD method for the determination of pollutants in model and real samples
• Author: Filip Dlačić
• Mentor: Danijela Ašperger (mentor)
• Committee member: Danijela Ašperger (predsjednik povjerenstva)
• Committee member: Davor Dolar (član povjerenstva)
• Committee member: Dragana Vuk (član povjerenstva)
• Granter: University of Zagreb; Faculty of Chemical Engineering and Technology; Zagreb
• Defense date and country: 2024-09-16, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Onečišćivala ljudskim djelovanjem dospijevaju u okoliš gdje se akumuliraju i zbog svoje toksičnosti predstavljaju problem za sve žive organizme. Danas ne postoji zakonska obveza praćenja koncentracija istih u okolišu, no trenutno se radi na tome da se uvedu i takve regulative pored postojanih pravilnika. Kako bi se omogućilo praćenje koncentracija i emisija onečišćivala u okolišu, potrebno je definirati pouzdanu metodu analize koja je primjenjiva za rad na svim uzorcima voda. Tekućinska kromatografija visoke djelotvornosti s detektorom s nizom dioda (HPLC-DAD) je kromatografska metoda analize koja je cjenovno vrlo pristupačna, brza i pouzdana metoda analize zbog svoje robusnosti, selektivnosti i osjetljivosti na niske koncentracije analita u uzorcima. Kromatografija se u biti dešava u koloni gdje dolazi do različitog zadržavanja analita na nepokretnoj odnosno u pokretnoj fazi što opet ovisi i o fizikalno-kemijskim svojstvima ne samo analita koji se određuje već i sorbensa u koloni te pokretnoj fazi. Međutim, jednom kada analiti prođu kroz kolonu sva redom odlaze na detektor s nizom dioda gdje se spektrofotometrijski detektiraju, a kao rezultat se dobivaju kromatogrami i apsorpcijski spektri za dobivanje kvantitativnih i kvalitativnih prametara za određivanje i detekciju ispitivanih analita. Da bi neka metoda mogla biti primjenjiva i pouzdana za određenu analizu ispitivanih analita, mora proći postupak validacije. Validacijom se određuju izvedbene značajke instrumenta i optimirane metode određujući parametre poput linearnosti, ponovljivosti, stabilnosti i iskoristivosti instrumentalne metode koji se zatim uspoređuju s definiranim kriterijima. U biti cilj postupka validacije je da se potvrdi je li izabrana i optimirana metoda prikladna za analizu ispitivanih analita u određenim uzorcima.

Abstract (english)

Contaminants introduced by human activities enter the environment, where they accumulate and pose a problem for all living organisms due to their toxicity. Currently, there is no legal obligation to monitor their concentrations in the environment, but efforts are underway to introduce such regulations alongside existing guidelines. To enable the monitoring of concentrations and emissions of contaminants in the environment, it is necessary to define a reliable analytical method applicable to all water samples. High-performance liquid chromatography with diode array detector (HPLC-DAD) is a chromatographic analysis method that is cost-effective, fast, and reliable due to its robustness, selectivity, and sensitivity to low concentrations of analytes in samples. Chromatography occurs primarily in the column, where analytes experience different retention times depending on their interactions with the stationary and mobile phases. These interactions are influenced by the physical and chemical properties of both the analytes and the stationary phase (sorbent) in the column, as well as the mobile phase. However, once the analytes pass through the column, they proceed to the diode array detector, where they are detected spectrophotometrically, resulting in chromatograms and absorption spectra that provide quantitative and qualitative parameters for the identification and detection of the analytes. For a method to be applicable and reliable for the analysis of specific analytes, it must undergo a validation process. Validation determines the performance characteristics of the instrument and the optimized method by assessing parameters such as linearity, repeatability, stability, and recovery of the instrumental method, which are then compared to defined criteria. Essentially, the goal of the validation process is to confirm whether the selected and optimized method is suitable for analyzing the target analytes in specific samples.

• Keywords: onečišćivala; kromatografija; validacija; HPLC-DAD
• Keywords (english): pollutants; chromatography; validation; HPLC-DAD
• Language: croatian
• URN:NBN: urn:nbn:hr:149:414502
• Project: Number: MYP-G6087; Title: Oporaba vode i membranski separacijski procesi za pouzdanu i održivu opskrbu vodom; Title: Water Reuse and Membrane Separation Processes for a Reliable and Sustainable Water Supply; Acronym: WaRMem; Leader: Davor Dolar; Jurisdiction: Belgium; Funder: Organizacija Sjevernoatlantskog sporazuma; Funding stream: Science for Peace and Security
• Study programme: Title: Chemical Engineering - Undergraduate study; Study programme type: university; Study level: undergraduate; Academic / professional title: sveučilišni/a prvostupnik/prvostupnica (baccalaureus/baccalaurea) inženjer/inženjerka kemijskog inženjerstva (sveučilišni/a prvostupnik/prvostupnica (baccalaureus/baccalaurea) inženjer/inženjerka kemijskog inženjerstva)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Embargoed access; Embargo expiration date: 2025-09-01
• Created on: 2024-11-15 13:03:08