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.

Comparison of triple quadrupole mass spectrometry and Orbitrap high‐resolution mass spectrometry in ultrahigh performance liquid chromatography for the determination of veterinary drugs in sewage: benefits and drawbacks

“…Glucocorticoids and polyether ionophores have been determined in sewage in previous papers [28,29] using UHPLC-MS/MS and LC-MS/MS methods, and these compounds were selected as candidates for the present study. Synthetic glucocorticoids and polyether ionophores are two examples of veterinary drugs that present an apparent ecotoxicological risk, [30][31][32][33] and their presence in surface waters, [28,29,[33][34][35][36][37][38][39][40][41][42][43][44] sewage, [28,29,33,34,[44][45][46][47][48][49] sewage sludge, [34,[49][50][51] soils, [40,[52][53][54][55][56] and sediments [38,39,44,52] has been reported.…”

Evaluation of two liquid chromatography/tandem mass spectrometry platforms for quantification of monensin in animal feed and milk

“…The fragmentation pattern of monensin depends on the precursor ion adducts and the dissociation mechanism 28, 3131, 43…”

A sensitive and validated HPLC–MS/MS method for simultaneous determination of seven coccidiostats in bovine whole milk

“…For all of the drugs, both positive and negative ESI were tested, but diclazuril was the only coccidiostat that required a negative ESI, these results were already reported by other authors who had analysed these substances in other matrices (Delahaut, Pierret, Ralet, Dubois, & Gillard, 2010;Dubois et al, 2004;Dubreil-Chéneau, Bessiral, Roudaut, Verdon, & Sanders, 2009;Vincent, Chedin, Yasar, & von Holst, 2008). As reported by Martínez-Villalba and collaborators, the sodium adduct of [M þ Na] þ for monensin, salinomycin, lasalocid, salinomycin, and narasin were employed as precursor ions (Martínez-Villalba, Moyano, & Galceran, 2009). The product ions selected were those that gave higher signal responses for the higher mass/charge ratio, [m/z] þ .…”