Fast liquid chromatography/multiple‐stage mass spectrometry of coccidiostats

Abstract

Drugs that are used as medicines and also as growth promoters in veterinary care are considered as emerging environmental contaminants and in recent years concern about their potential risk to ecosystems and human health has risen. In this paper we used a method based on liquid chromatography/electrospray tandem mass spectrometry to analyze eight coccidiostatic compounds: diclazuril, dinitrocarbanilide (the main metabolite of nicarbazin), robenidine, lasalocid, monensin, salinomycin, maduramicin and nasarin. Multiple-stage mass spectrometry (MSn) based on the precursor ions [M+Na]+ (polyether ionophores), [M+H]+ (robenidine) and [M-H]- (diclazuril and dinitrocarbanilide) was used to study the fragmentation of these compounds. MSn data and genealogical relationships were used to propose a tentative assignment of the different fragment ions. Loss of water, decarboxylations, ketone beta-cleavages and rearrangement of cyclic ethers and amide groups were some of the fragmentations observed for these compounds. Liquid chromatography with a sub-2 microm particle size column was coupled to tandem mass spectrometry (LC/MS/MS) allowing the separation of these compounds in less than 7 min. Method detection limits ranging from 11 to 71 ng L(-1) and run-to-run values in terms of relative standard deviation (RSD) (up to 12%) were obtained.