| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1199781 | Journal of Chromatography A | 2014 | 12 Pages |
•Development of new rapid analytical method for 22 compounds of sulfonamides and their metabolites.•Combination QuEChERS–LC–LTQ-Orbitrap was applied.•A comprehensive qualitative and quantitative method was proposed.•Full validation of proposed method according to 2002/657/EC decision criteria.•Method was applied to a certified reference material and real animal tissues samples.
A new high performance liquid chromatography–high resolution mass spectrometry (HPLC–HRMS) method was developed for a simultaneous multi-residue analysis of 22 sulfonamides (SAs) and their metabolites in edible animal (pig, beef, sheep and chicken) tissues. Sample preparation was optimized on the basis of the “QuEChERS” protocol. The analytes were identified using their LC retention times and accurate mass; the identification was further confirmed by multi-stage high mass accuracy (<5 ppm) mass spectrometry. The performance of the method was evaluated according to the EU guidelines for the validation of screening methods for the analysis of veterinary drugs residues. Acceptable values were obtained for: linearity (R2 < 0.99), limit of detection (LOD, 3–26 μg/kg), limit of quantification (LOQ, 11–88 μg/kg), accuracy (recovery 88–112%), intra- and inter-day precision 1–14 and 1–17%, respectively, decision limit (CCα) and detection capability (CCβ) around the maximum residue limits (MRL) of SAs (100 μg/kg). The method was validated by analysis of a reference material FAPAS-02188 “Pig kidney” with ǀ Z-scoreǀ < 0.63. The method was applied to various matrices (kidney, liver, muscle) originated from pig, beef, sheep, and chicken) allowing the simultaneous quantification of target sulfonamides at concentration levels above the MRL/2 and the identification of untargeted compounds such as N4-acetyl metabolites using multi-stage high mass accuracy mass spectrometry.
