Animal feeding stuffs. Methods of sampling and analysis. Determination of pyrrolizidine alkaloids in animal feeding stuff by LC-MS/MS

Animal feeding stuffs. Methods of sampling and analysis. Determination of pyrrolizidine alkaloids in animal feeding stuff by LC-MS/MS

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1   Scope

This document specifies a method for the quantitative determination of pyrrolizidine alkaloids (PA) in the concentration ranges shown in Table 1 in complete and supplementary feed and in forages by liquid chromatography tandem mass spectrometry (LC-MS/MS) after solid phase extraction (SPE) clean-up.
Table 1 — Summary of concentration ranges per PA tested in the collaborative trial
Tested pyrrolizidine alkaloid (PA) Abbreviation Tested concentration range a (µg/kg)
From To
Echimidine Em 20 435
Echimidine-N-oxide EmN 5 30
Erucifoline Er 20 245
Erucifoline-N-oxide ErN 20 370
Europine Eu 15 330
Europine-N-oxide EuN 25 285
Heliotrine Hn 25 280
Heliotrine-N-oxide HnN 25 245
Jacobine Jb 20 230
Jacobine-N-oxide JbN 20 215
Lasiocarpine Lc 20 350
Lasiocarpine-N-oxide LcN 5 250
Intermedine Im 25 560
Intermedine-N-oxide ImN 5 395
Lycopsamine La 25 500
Lycopsamine-N-oxide LaN 20 280
Monocrotaline Mc 20 360
Monocrotaline-N-oxide McN 20 365
Retrorsine Re 250 375
Retrorsine-N-oxide ReN 5 285
Senecionineb Sc 25 205
Senecionine-N-oxide b ScN 5 300
Senecivernine b Sv 20 205
Senecivernine-N-oxide b SvN 5 165
Senkirkine Sk 20 275
Seneciphylline Sp 25 225
Seneciphylline-N-oxide SpN 5 225
Trichodesmine Td 5 250
Intermedine + Lycopsamine Im+La 50 890
Intermedine-N-oxide + Lycopsamine-N-oxide ImN+LaN 5 645
Senecivernine + Senecionine Sv+Sc 30 280
Senecivernine-N-oxide + Senecionine-N-ide SvN+ScN 10 380
a Rounded figures
b Individual PA of the isomeric pairs Sv+Sc and SvN+ScN were not evaluated statistically due to insufficient chromatographic separation.

NOTE 1 A second method was part of the method validation collaborative main trial. For this method PA-N-Oxides are reduced by adding zinc powder to the extract of the feed material. The following steps correspond to the first and main method. Quantitative results for each PA except the otonecine type PA senkirkine represent the sum of the free PA base and its corresponding N-oxide.

NOTE 2 Due to insufficient numbers of data for some analyte-matrix combinations statistical evaluation was not valid for standardization. Received data indicated the methods applicability in experienced laboratories with appropriate quality assurance measures. Therefore, the method description is included as an informative annex (Annex D).