Skip to Content
Merck
  • UPLC-MS/MS method for determination of selected pyrrolizidine alkaloids in feed.

UPLC-MS/MS method for determination of selected pyrrolizidine alkaloids in feed.

Food chemistry (2014-10-13)
Martina Bolechová, Josef Cáslavský, Markéta Pospíchalová, Petra Kosubová
ABSTRACT

Alkaloids known as secondary metabolites are grouped by typical structural characteristics into large families such as pyrrolizidine alkaloids (PAs) comprising more than 350 individual heterocyclic compounds. The PAs present a serious health risk to human and livestock; hence there is a need for methods that allow these dangerous plant toxins to be determined. In this study, a fast, reliable and sensitive approach is proposed to identify and quantify PAs in feed samples. PAs including monocrotaline, senkirkine, senecionine, seneciphylline and retrorsine were determined by ultra-performance liquid chromatography coupled with tandem mass spectrometry. Sample preparation was based on a modified QuEChERS approach. The mean recovery, precision, matrix effects and limits of quantification were assessed for three matrices within the method validation. The presented method was used to inspect 41 various feed samples, where the presence of PAs was expected. Roughages and feed for rabbits contained the highest levels of PAs, in general.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Formic acid solution, BioUltra, 1.0 M in H2O
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Crotaline
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Acetonitrile, HPLC Plus, ≥99.9%
Sigma-Aldrich
Acetonitrile, ACS reagent, ≥99.5%