Fast liquid chromatography/tandem mass spectrometry (highly selective selected reaction monitoring) for the determination of toltrazuril and its metabolites in food

Abstract

In this work a fast liquid chromatography (LC)-tandem mass spectrometry (MS/MS) method was developed for the analysis of toltrazuril, a coccidiostatic drug, and its metabolites in meat food products. The applicability of atmospheric pressure chemical ionization (APCI) and heated electrospray ionization in both positive and negative modes was studied. APCI in negative mode provided the best results and the base peak originated from the loss of CF(3) (toltrazuril and toltrazuril sulfone) and CHF(3)* (toltrazuril sulfoxide) was used as the precursor ion in MS/MS. A fast LC separation on a C(18) Fused-Core column was used together with the APCI-MS/MS method developed using enhanced mass resolution mode (highly selective selected reaction monitoring, H-SRM) to improve the sensitivity and selectivity for the analysis of these compounds in food samples. A simple sample treatment based on an extraction with acetonitrile and a cleanup with a C(18) cartridge was used. The LC-MS/MS (H-SRM) method showed good precision (relative standard deviation lower than 10%), accuracy, and linearity and allowed the determination of these compounds in food samples down to the parts per billion level (limits of detection between 0.5 and 5 microg kg(-1)).

Determination of diclazuril, toltrazuril and its two metabolites in poultry tissues and eggs by gel permeation chromatography–liquid chromatography–tandem mass spectrometry

“…Croubels et al [7] described a LC-MS/MS for the detection of DIZ in animal plasma with a LOQ of 1 g/L and a LC-MS/MS for the detection of DIZ in poultry meat and feed with CC␣ and CC␤ values of 0.5 and 0.6 g/kg was developed by Mortier et al [8]. There are also some multiresidue LC-MS/MS methods to detect coccidiostats including DIZ and TOZ in chicken tissues and eggs [9][10][11][12][13]. However, there has been no report of simultaneous analysis of DIZ, TOZ, and its two metabolites (TZSO and TZS) in poultry tissues and eggs.…”

“…Several methods for the determination of DIZ or TOZ in feed, biological fluids, animal tissues and eggs have been reported [5][6][7][8][9][10][11][12][13]. A LC method for the simultaneous determination of the residues of DIZ and TOZ in chicken tissues was developed using matrix solidphase dispersion (MSPD) for clean-up, and the LOQs of DIZ and TOZ were 10 and 12 g/kg for muscle, respectively, and 15 g/kg for liver and kidney [5].…”

A multi‐residue method for 17 anticoccidial drugs and ractopamine in animal tissues by liquid chromatography‐tandem mass spectrometry and time‐of‐flight mass spectrometry

“…Methods using acetonitrile where the crude extract was evaporated, re‐dissolved, and injected into the mass spectrometry system were found not to be optimum for liver tissues . Other methods used acetonitrile as an extraction solvent, with additional solid phase extraction clean up, using silica SPE or C 18 SPE . Another method using acetonitrile as the extraction solvent, then directly injecting the extract required additional sample clean up depending on the matrix …”

“…[5][6][7] Other methods used acetonitrile as an extraction solvent, with additional solid phase extraction clean up, using silica SPE or C 18 SPE. [8,9] Another method using acetonitrile as the extraction solvent, then directly injecting the extract required additional sample clean up depending on the matrix. [10]…”

Liquid Chromatography Tandem Mass Spectrometry Analysis of Synthetic Coccidiostats in Eggs

“…At the moment, there are few papers about toltrazuril and its metabolites in eggs or in feedstuffs [30][31][32] and, to our knowledge, there are no scientific works about these five synthetic coccidiostats and the toltrazuril metabolites all together.…”