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Multi‐drug ultraperformance liquid chromatography/tandem mass spectrometry method to quantify antimicrobials in feeding stuffs at carry‐over level
Author(s) -
Civitareale Cinzia,
Mestria Serena,
Gallo Pasquale,
Giannetti Luigi,
Neri Bruno,
Stacchini Paolo,
Fiori Maurizio
Publication year - 2018
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.8216
Subject(s) - chemistry , chromatography , detection limit , analyte , oxytetracycline , tandem mass spectrometry , veterinary drug , spiramycin , veterinary drugs , liquid chromatography–mass spectrometry , mass spectrometry , antibiotics , erythromycin , veterinary medicine , medicine , biochemistry
Rationale Carry‐over is an undesirable contamination from medicated to non‐medicated during the production of feedingstuffs. In 2014 the European Parliament and the Council started working to produce a new regulatory act that will fix tolerable levels of drugs by carry‐over in non‐target feed to have a harmonized practice to evaluate this contamination by veterinary drugs. Methods We developed a rapid and effective multi‐analyte method coupling ultraperformance liquid chromatography to tandem mass spectrometry (UPLC/MS/MS) for the detection of 37 drugs belonging to different classes of antimicrobials (sulfonamides, tetracyclines, macrolides, quinolones, pleuromutilins and streptogramins) in feeds at carry‐over levels. The method was in‐house validated in the concentration range 0.25–2.0 mg kg −1 , according to the Regulation (UE) 2017/625 requirements and the guideline included in the Commission Decision 2002/657/EC for official methods. Results The UPLC/MS/MS method allows the determination of the antimicrobials in 15 min, by providing results compliant to the criteria established by the European Commission legislation. All the analytes showed a limit of detection (LOD) in the range 2.0–5.0 μg kg −1 and a limit of quantification (LOQ) at 10.0 μg kg −1 ; oxytetracycline, doxycycline, spiramycin and virginiamycin have a higher LOD and LOQ (15.0 μg kg −1 ; 30.0 μg kg −1 , respectively). Recoveries were satisfactory ranging from 90.4% to 103.1%. Conclusions The method is characterized by an effective clean‐up of all drugs without the use of large sample size and organic solvent extraction.