4.7 Article

Development and validation of a multiclass method for the determination of veterinary drug residues in chicken by ultra high performance liquid chromatography-tandem mass spectrometry

Journal

TALANTA
Volume 89, Issue -, Pages 201-208

Publisher

ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2011.11.082

Keywords

Multiclass analysis; Chicken; Veterinary drug residues; QuEChERS; UHPLC-MS/MS; Validation

Funding

  1. Spanish Ministry of Science and Innovation (MICINN)-FEDER [AGL2010-21370]
  2. National Council for Scientific and Technological Development (CNPq)-Brazil
  3. SMSI-ESF

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A multiclass method has been optimized and validated for the simultaneous determination of 20 veterinary drug residues belonging to several classes, as quinolones, sulfonamides, macrolides, anthelmintics, avermectins and diamino derivatives, and benzathine, used as a marker of the presence of penicillin, in muscle chicken. It has been based on QuEChERS methodology (quick, easy, cheap, effective, rugged and safe) and ultra high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UHPLC-MS/MS). Several chromatographic conditions were optimized, obtaining a running time <8.5 min. The developed method was validated on the basis of international guidelines. Mean recoveries ranged from 70 to 120%, except for benzathine (65.6% at 20 mu g kg(-1)) and sulfadimidine (69.0% at 100 mu g kg(-1)). Repeatability was lower than 20.0% except for sulfachlorpyridazine (22.1% at 20 mu g kg(-1)) and tylosin (20.5% and 20.6% at 30 and 50 mu g kg(-1), respectively), whereas reproducibility was lower than 25% except for flumequine (27.4% at 20 mu g kg(-1)) and benzathine (37.8% and 27% at 20 and 50 mu g kg(-1), respectively). Limits of detection (LODs) and quantification (LOQs) ranged from 3.0 to 6.0 mu g kg(-1) and 10.0 to 20.0 mu g kg(-1), respectively, except for tylosin that showed a LOD and LOQ of 9.0 and 30.0 mu g kg(-1). Decision limit (CC alpha) and detection capability (CC beta) were calculated and CC beta ranged from 24.1 mu g kg(-1) (mebendazole) to 423.6 mu g kg(-1) (flumequine). Finally, the method was applied to real samples and traces of some compounds were found in eight samples of chicken and benzathine was detected in one sample at 29.9 mu g kg(-1). (C) 2011 Elsevier B.V. All rights reserved.

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