title: Determination of monensin, narasin, and salinomycin in mineral premixes, supplements, and animal feeds by liquid chromatography and post-column derivatization: collaborative study.
abstract: A liquid chromatographic (LC) method for the analysis of monensin, narasin, and salinomycin in mineral premixes, supplements, and complete animal feeds at medicating and trace levels was collaboratively studied. The method uses methanol-water (90 + 10) extraction with mechanical shaking for 1 h, filtration, and dilution if necessary. Determination of the 3 ionophores is by reversed-phase LC using post-column derivatization with vanillin and detection at 520 nm. Suspect positive trace-level products and medicated feeds containing unexpected ionophores are confirmed by hexane extraction or post-column derivatization with dimethylaminobenzaldehyde (DMAB). Twenty-five test samples of medicated feeds, supplements, and mineral and drug premixes, and 9 test samples for trace-level analysis were sent to 11 collaborators in Bulgaria, Czech Republic, Portugal, France, The Netherlands, United States, and Canada. Acceptable results were received from 10 laboratories. For the medicated complete feeds, supplements, and mineral premixes, RSDr values (within-laboratory repeatability) ranged from 2.5 to 5.2%, RSDR values (among-laboratory reproducibility) ranged from 2.7 to 6.8%, and HorRat values ranged from 0.31 to 1.30. For the drug premixes, the result variability was excessive and HorRat values ranged from 2.27 to 14.1. For the trace-level test samples, all laboratories correctly identified the analytes and did not report any false positives. RSDr values ranged from 1.3 to 9.5%, RSDR values ranged from 5.2 to 13.1%, and HorRat values ranged from 0.4 to 0.97.
authors.affiliation: Canadian Food Inspection Agency, Ottawa Laboratory (Carling), Ottawa, ON, Canada. hcampbell@inspection.gc.ca
authors.forename: Harold
authors.initials: H
authors.lastname: Campbell
authors.forename: Gita
authors.initials: G
authors.lastname: Nayeri
mesh_terms: D000821:Animal Feed / Q000032:analysis*; D000900:Anti-Bacterial Agents / Q000032:analysis*; D001547:Benzaldehydes; D002853:Chromatography, Liquid / Q000379:methods* / Q000592:standards / Q000706:statistics & numerical data; D003299:Cooperative Behavior; D019587:Dietary Supplements / Q000032:analysis*; D007202:Indicators and Reagents; D008985:Monensin / Q000032:analysis*; D011714:Pyrans / Q000032:analysis*; D015203:Reproducibility of Results; D000095662:Polyether Polyketides
chemical_list: D000900:Anti-Bacterial Agents; D001547:Benzaldehydes; D007202:Indicators and Reagents; D008985:Monensin; D011714:Pyrans; C010327:salinomycin; D000095662:Polyether Polyketides; C100058:vanillin; C013612:narasin; C510241:p-dimethylaminobenzaldehyde