Analysis of steroidal compounds in wastewater by liquid chromatography-mass spectrometry : comparison of different ionization techniques

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http://urn.fi/URN:NBN:fi-fe2017112251611
Title: Analysis of steroidal compounds in wastewater by liquid chromatography-mass spectrometry : comparison of different ionization techniques
Author: Lizcano, Raymundo
Contributor: University of Helsinki, Faculty of Science, Department of Chemistry
Publisher: Helsingfors universitet
Date: 2013
Language: eng
URI: http://urn.fi/URN:NBN:fi-fe2017112251611
http://hdl.handle.net/10138/230567
Thesis level: master's thesis
Discipline: Analytical Chemistry
Analyyttinen kemia
Analytisk kemi
Abstract: In the literature part an introduction to emerging organic contaminants is presented as well as the subcategory of endocrine disrupting chemicals, which includes steroid hormones. An overview of liquid chromatography trends in environmental analysis as well as mass spectrometry operational conditions are discussed. Review is focused on ionization techniques and tandem mass spectrometry functionalities reported on state of the art studies of steroidal compounds in environmental samples. Experimental part presents an extensive sample preparation method and a liquid chromatography – mass spectrometry (HPLC-MS) method that were developed for the determination of concentration of eleven steroidal compounds: 4-androstene-3,17-dione (A1), trans-androsterone (A2), Corticosterone (C1), Cortisone (C2), Estrone (E1), 17-β-estradiol (E2), Estriol (E3), 17-α-ethynil estradiol (EE2), Progesterone (P), 17-hydroxy progesterone (HP) and Testosterone (T). Separation efficiency and analysis time were compared for three HPLC columns with different stationary phase: Pentafluorophenyl (PFP), C8 and C18 monolithic. Three atmospheric pressure ionization (API) techniques were tested to compare their performance: Electrospray ionization (ESI), Atmospheric Pressure Chemical Ionization (APCI) and Atmospheric Pressure Photoionization (APPI). The proposed method included the best column choice coupled with the API technique, which presented an efficient ionization for most of the target analytes. Best methodology was applied to the analysis of effluent and influent samples from the wastewater treatment plant in Viikinmäki, Helsinki.


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