Mikrovalno potpomognuta ekstrakcija polibromiranih difenil etera iz ljudskog mlijeka

master's thesis

• Title (english): Microvawe-assisted extraction of polybrominated diphenyl ethers from human milk
• Author: Lucija Besednik
• Mentor: Darija Klinčić (mentor)
• Committee member: Nives Galić (predsjednik povjerenstva)
• Committee member: Morana Dulić (član povjerenstva)
• Committee member: Željka Soldin (član povjerenstva)
• Committee member: Adriana Kenđel (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2020-09-18, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

Razrađeni su uvjeti ekstrakcije potpomognute mikrovalovima (MAE) za polibromirane difenil
etere (PBDE) iz uzoraka ljudskog mlijeka. Istražen je utjecaj načina pripreme uzorka te su
optimirani uvjeti tehnike MAE (vrsta i volumen otapala, temperatura ekstrakcije). Pročišćeni
ekstrakti analizirani su plinskom kromatografijom uz detektor zahvata elektrona. Tehnika
MAE pokazala je zadovoljavajuću djelotvornost za ekstrakciju spojeva PBDE iz uzoraka
ljudskog mlijeka u tekućem stanju, dok u slučaju liofiliziranog uzorka mlijeka nije bila
djelotvorna. Postupak ekstrakcije spojeva PBDE tehnikom MAE iz liofiliziranog ljudskog
mlijeka otopljenog u ultračistoj vodi smjesom otapala φ (n-heksan, aceton) = 1:1 uz dodatak
mravlje kiseline i propan-2-ola pri temperaturi od 80 °C tijekom 20 minuta izdvojen je kao
najprikladniji. Analitički povrat spojeva bio je u rasponu od 61 % za BDE-47 do 83 % za
BDE-183, uz relativnu standardnu devijaciju 7 %. U uzorku korištenom za razradu metode
analiziranom bez dodatka analita pri odabranim uvjetima detektiran je samo BDE-153
(0,19 ng g–1 masti).

Abstract (english)

Microwave-assisted extraction (MAE) procedures for polybrominated diphenyl ethers (PBDEs) from
human milk samples have been studied. The influence of the sample preparation method was
investigated and the conditions of the MAE technique (type and volume of solvent, extraction
temperature) were optimized. The purified extracts were analyzed by gas chromatography with an
electron capture detector. The MAE technique has shown satisfactory efficiency for the extraction of
PBDEs from liquid milk samples, while in the case of a lyophilized milk sample it was not effective.
The process of extraction of PBDEs by MAE technique from lyophilized human milk dissolved in
ultrapure water with a mixture of solvent φ (n-hexane, acetone) = 1: 1 with the addition of formic acid
and propan-2-ol at a temperature of 80 ° C for 20 minutes was selected as the most suitable.
Analytical recoveries of selected analytes ranged from 61 % for BDE-47 to 83 % for BDE-183, with a
relative standard deviation of 7 %. In the sample used for method development, analyzed without the
addition of analytes under selected conditions, only BDE-153 was detected (0,19 ng g–1 lipid).

• Keywords: ekstrakcija potpomognuta mikrovalovima; ljudsko mlijeko; plinska kromatografija; polibromirani difenil eteri
• Keywords (english): gas chromatography; human milk; microwave-assisted extraction; polybrominated diphenyl ethers
• Language: croatian
• URN:NBN: urn:nbn:hr:217:789551
• Study programme: Title: Graduate university studies in chemistry; specializations in: Research programme; Course: Research programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access; Embargo expiration date: 2022-09-18
• Created on: 2020-10-07 08:57:08