Development and Validation of Confirmatory Methods for Determining Prohibited Substances in Urine of Horses with Technical UPLC-QTOFMS, for Doping Control

Postgraduate Thesis uoadl:1315897 593 Read counter

Unit:
Κατεύθυνση Αναλυτική Χημεία
Library of the School of Science
Deposit date:
2016-02-17
Year:
2016
Author:
Φωτεινοπούλου Ηλέκτρα
Supervisors info:
Θωμαΐδης Νικόλαος Αναπλ. Καθηγητής (επιβλέπων), Κουππάρης Μιχαήλ Καθηγητής, Οικονόμου Αθανάσιος Αναπλ. Καθηγητής
Original Title:
Ανάπτυξη και Επικύρωση Επιβεβαιωτικών Μεθόδων Προσδιορισμού Απαγορευμένων Ουσιών σε Ούρα Αλόγων με την Τεχνική UPLC-QTOFMS, για τον Έλεγχο Ντόπινγκ
Languages:
Greek
Translated title:
Development and Validation of Confirmatory Methods for Determining Prohibited Substances in Urine of Horses with Technical UPLC-QTOFMS, for Doping Control
Summary:
This Master Thesis, conducted in doping control laboratory of the Olympic
Stadium in Athens, in collaboration with the University of Athens, presents the
development and validation of confirmatory methods for the detection of banned
substances in horse urine using Liquid Chromatography – Mass Spectrometry and
the use of a Time of Flight mass analyzer coupled with a quadrupole (LC-QTOF).
Analytes where ionized with an electrospray ionization, performed in the
positive mode [(+)ESI]. For the development we followed the following strategy:
At first multicomponent solutions containing large number of prohibited
substances were analyzed by LC-QTOF, at full ion scan (full scan), to find the
retention time and the relative retention time and main ions that appear in the
mass spectrum of substances. Then, studies were conducted to optimize the
dynamic of the ionization source in order to optimize the signal to determine
the 90 banned substances. This was followed by a study finding the optimum
collision energy values, in order to have at least 2 diagnostics fragments for
each substance. Finally specialized analysis and printing methods were built
for each of the restricted substances tested. To validate the method, a number
of parameters examined for 10 representative substances. The evaluation of the
confirmation method, showed that this method exhibits specificity for all the
substances tested. In addition, not any carry over nor matrix interferences
have been observed in the analyzed samples. Finally, a recording of spectra was
held in the body of the electronic library.
Keywords:
Liquid chromatography (LC), Mass spectrometry (MS), Time of flight (TOF), Horse urine, Peptides
Index:
No
Number of index pages:
15, 17, 19
Contains images:
Yes
Number of references:
64
Number of pages:
153
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