Liquid chromatography-tandem mass spectrometry characterization of ergocristam degradation products.
The UPLC method with diode array UV detection was developed for qualitative determination of ergocristine and ergocristam including degradation products. The mechanism of the ergocristam disruptive reaction was described based on MS/MS characterization of ammonolytic product, N-(d-lysergyl)-l-valinamide (A1) and two methanolytic products, methyl ester of N-(d-lysergyl)-l-valine (M2), and N-[N-(d-lysergyl)-l-valyl]-l-phenylalanyl-d-prolyl methyl ester (M1). The influence of extraction conditions on epimerization and degradation of ergocristine and ergocristam was tested and conditions for reproducible decomposition of ergocristam were found. The presented method could potentially be applied for ergot alkaloids determination in sclerotia, fermentation broth, mycelium, and possibly contaminated food products, i.e. corn, flour, bread, etc., and feeding stuffs containing ungrounded cereals.
Olsovská
Jana
J
Institute of Microbiology Academy of Sciences of the Czech Republic, v.v.i., Vídenská 1083, 14220 Prague 4, Czech Republic.
Sulc
Miroslav
M
Novák
Petr
P
Pazoutová
Sylvie
S
Flieger
Miroslav
M
D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004873:Ergolines / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D004876:Ergot Alkaloids / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D005506:Food Contamination / Q000032:analysis*; D053719:Tandem Mass Spectrometry / Q000379:methods*
D004873:Ergolines; D004876:Ergot Alkaloids; C100270:ergocristine