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Structural characterization of fatty acids with triple bond and unusual double bond positions by HPLC/APCI-MS2
Horká, Petra ; Vrkoslav, Vladimír ; Cvačka, Josef
Fatty acid methyl esters (FAMEs) were analyzed by reversed-phase HPLC coupled to atmospheric pressure chemical ionization (APCI) mass spectrometry. Acetonitrile was used as mobile phase. The gas-phase reactions of acetonitrile and unsaturated FAMEs in the APCI source provided [M + C3H5N]+• adducts. Subsequent MS/MS analysis of these ions gave diagnostic fragments. The formation and fragmentation of the acetonitrile-related adducts were utilized for the structural characterization of FAME with isolated double bonds in (Z)-9,19-hexacosadienoic acid methyl ester, FAME with conjugated double bonds in (Z)-9,11-octadecadienoic acid methyl ester and FAME with a triple bond in 9-octadecynoic acid methyl ester.
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Method optimization for simultaneous separation of six triazole fungicides in HPLC
Kovač, Ishak ; Martín Miján, P. ; Del Sol Vega Alegre, M. ; Dejmková, H. ; Jaklová Dytrtová, Jana ; Schwarzová, K.
Triazole pesticides are widely used in agriculture against fungi pathogens. Their application is not restricted on just one member of the group, more importantly, the application is usually carried out in the mixture of two or more triazoles. Hence, this work focuses on simultaneous separation and detection of six triazole fungicides: penconazole, tebuconazole, propiconazole, cyproconazole, fenbuconazole, and difenoconazole. Two different columns were tested with different parameters for isocratic and gradient elution in HPLC with UV detector. On Purospher Reverse Phase-18 column with gradient elution isomers of triazoles cyproconazole and propiconazole were successfully separated. However, on this column, there was an overlap of some triazoles. In contrast, the isocratic elution on Kromasil Eternity-5-PhenylHexyl column showed sufficient separation capabilities. In further research, chiral separation of triazoles will be considered using capillary electrophoresis.
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