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Čiščenje ekstraktov trdnih vzorcev s HFME
ID Uranič, Ajda (Author), ID Prosen, Helena (Mentor) More about this mentor... This link opens in a new window

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Abstract
Benzotriazoli so organske spojine, njihova uporaba je zelo razširjena na različnih področjih. Posledica razširjene uporabe je, da se pojavljajo v okolju kot onesnaževala. Za določanje benzotriazolov v okoljskih matricah lahko uporabimo različne metode, kot npr. SPE oz. ekstrakcijo na trdno fazo in nato tekočinsko kromatografijo ali plinsko kromatografijo. V zadnjem obdobju pa se razvijajo predvsem metode, prijazne do okolja. Ena izmed njih je tudi mikroekstrakcija z votlim vlaknom (HFME). Metoda je preprosta, poceni in daje zelo čiste ekstrakte. Namen diplomskega dela je bilo čiščenje ekstraktov trdnih vzorcev s HFME in določitev benzotriazolov s tekočinsko kromatografijo visoke ločljivosti (HPLC). Pri preizkusu HFME sem določila obogatitvene faktorje (EF) analitov, ekstrakcija je dala dobre rezultate pri vseh analitih. Z ekstrakcijo ekstrakta tal sem ugotovila, da dodatek manjše količine (0,2 % v raztopini vzorca) raztopine EDTA znatno poveča obogatitvene faktorje vseh analitov. Z ekstrakcijo vzorca tal sem ocenila, da je meja zaznave analitov 1 mg/kg. Nato sem določila vpliv acetona na učinkovitost ekstrakcije in na ekstrakcijo ekstrakta tal. Majhen delež acetona je pozitivno vplival na uspešnost ekstrakcije, pri 0,5 % acetona v raztopini se je obogatitveni faktor povečal pri vseh analitih. Pri povečevanju deleža acetona pa se faktorji obogatitve zmanjšujejo. Sledila je določitev s HPLC. Na koncu sem ugotavljala, ali lahko z izbrano metodo benzotriazole določim tudi v realnih vzorcih. V vzorcih anaerobnega in aerobnega blata iz biološke čistilne naprave sem z metodo standardnega dodatka potrdila prisotnost 4-hidroksi-1H-benzotriazola v obeh vzorcih. V vzorcu anaerobnega blata je njegova koncentracija znašala vsaj 6,7 ng/g s.s., v vzorcu aerobnega blata pa vsaj 5,9 ng/g s.s..

Language:Slovenian
Keywords:benzotriazoli, mikroekstrakcija z votlim vlaknom (HFME), tekočinska kromatografija visoke ločljivosti (HPLC)
Work type:Bachelor thesis/paper
Typology:2.11 - Undergraduate Thesis
Organization:FKKT - Faculty of Chemistry and Chemical Technology
Year:2020
PID:20.500.12556/RUL-117842 This link opens in a new window
COBISS.SI-ID:23456771 This link opens in a new window
Publication date in RUL:29.07.2020
Views:2127
Downloads:208
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Secondary language

Language:English
Title:Clean-up of solid samples extracts with HFME
Abstract:
Benzotriazoles are organic compounds and their use is widespread in various fields. As a consequence of their widespread use, they appear in the environment as pollutants. Various methods can be used to determine benzotriazoles in environmental matrices, such as SPE or solid phase extraction with liquid chromatography or gas chromatography. Recently, environmentally friendly methods have been developed. One of them is Hollow Fiber Microextraction (HFME). The method is simple, inexpensive and gives very pure extracts. The aim of this study was to purify extracts of solid samples with HFME and to determine benzotriazoles by high-performance liquid chromatography (HPLC). I performed HFME test and determined the enrichment factors (EF), the extraction was successful for all analytes. By the extraction of the soil extract, I found that the addition of a smaller amount (0.2 % in the sample solution) of EDTA solution significantly increased the enrichment factors of all analytes. For the extraction of the soil extract, I astimated that the limit of detection was 1 mg/kg. Then I determined the effect of acetone on the efficiency of the extraction and on the extraction of the soil extract. A small fraction of acetone had a positive effect on the extraction, with 0.5 % acetone in solution increasing the enrichment factor in all analytes. As the fraction of acetone increased, the enrichment factors decreased. Determination by HPLC followed. In the end I established whether determination of benzotriazoles in real samples with the chosen method is possible. In the samples of anaerobic and aerobic sludge from the biological treatment plant, I confirmed the presence of 4-hydroxy-1H-benzotriazole in both samples using the method of standard addition. Its concentration was at least 6.7 ng/g d.m. in the anaerobic sludge sample and at least 5.9 ng/g d.m. in the aerobic sludge sample.

Keywords:benzotriazoles, hollow fiber microextraction (HFME), high-performance liquid chromatography (HPLC)

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