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Development of UHPLC-MS/MS and UHPSFC-MS/MS methods for determination of selected ochratoxins
Kretek, Kristián ; Nováková, Lucie (advisor) ; Chmelařová, Hana (referee)
Charles University, Faculty of Pharmacy in Hradec Králové Department of Analytical Chemistry Candidate: Kristián Kretek Supervisor: prof. PharmDr. Lucie Nováková, Ph.D. Title of the diploma thesis: Development of UHPLC-MS/MS and UHPSFC-MS/MS methods for determination of selected ochratoxins The purpose of this work was development and comparison of UHPLC and UHPSFC analytical methods coupled to tandem mass spectrometry for four common ochratoxins. The experiments were performed using UHPLC system ACQUITY UPLC and UHPSFC system ACQUITY UPC2, mass spectrometer XEVO TQ-XS was the same in both cases. First, optimization of ion source parameters and SRM transitions was done. For UHPLC along with ACN, 3 additives of the water-based component of mobile phase were tested - formic, acetic acid and ammonia, with flow rate 0,4 ml/min, gradient from 2 % to 95 % ACN in 5th minute, temperature 40řC and column Acquity UPLC BEH C18. For UHPSFC 6 organic modifiers along with CO2 were tested: MeOH and MeOH with addition of water, formic acid, ammonia, and ammonium formate, with flowrate 1,5 ml/min, gradient from 2 % to 45 % MeOH in 5th minute, temperature 40řC and BPR pressure 2000 psi. Screening of 13 columns was also conducted. Optimization of MS detection in SFC was done by testing 8 make-up solvents: MeOH, EtOH,...
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