title: Determination of pyrrolizidine alkaloids in selected feed materials with gas chromatography-mass spectrometry.
abstract: 1,2-Dehydropyrrolizidine alkaloids are known to be toxic to many animals and humans. To provide safety of feeds a method based on gas chromatography-mass spectrometry enabling the determination of a content of 1,2-unsaturated PAs in feed materials was developed. After extraction with aqueous solution of HCl and purification of the extract, 1,2-unsaturated alkaloids are reduced to their common backbone structures and subsequently derivatised with heptafluorobutyric anhydride (HFBA). The method was validated according to SANTE/11945/2015. All received parameters are consistent with the document requirements as recovery of a final compound retronecine derivative was from 81.8% to 94.4% when retrosine was used for spiking and from 72.7% to 85.5% when retrorsine N-oxide was spiked. The repeatability was calculated as relative standards deviation and ranged from 7.5% to 14.4%, for N-oxide was from 7.9% to 15.4%. The reproducibility was in the range from 14.2% to 16.3% and from 17.0% to 18.1% for free base and N-oxide respectively. The limit of quantification was determined as 10 µg kg-1. Good linearity of the method was obtained with coefficient of determination R2> 0.99. The method was applied to 35 silage and two hay samples analysis.
authors.affiliation: a Department of Hygiene of Animal Feedingstuffs , National Veterinary Research Institute , Puławy , Poland.
authors.forename: Ewelina
authors.initials: E
authors.lastname: Kowalczyk
authors.affiliation: a Department of Hygiene of Animal Feedingstuffs , National Veterinary Research Institute , Puławy , Poland.
authors.forename: Krzysztof
authors.initials: K
authors.lastname: Kwiatek
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000818:Animals; D059022:Food Safety; D008401:Gas Chromatography-Mass Spectrometry; D011763:Pyrrolizidine Alkaloids / Q000032:analysis*
chemical_list: D011763:Pyrrolizidine Alkaloids
keywords: GC-MS method; Pyrrolizidine alkaloids; animal feed; hay; silage