Journal of Food, Agriculture and Environment

Method optimization and performance characteristics for the determination of twelve veterinary drugs in food of animal origin using modified QuEChERS and LC-MS/MS QTRAP detection


Mahmoud Abd Elkhabeer 1, 4*, Gouda A. Ramadan Gouda 1, 2, Lamia Ryad 2, Najat Alabdulmalik 1,  Eglal R. Souaya 3

Recieved Date: 2019-01-07, Accepted Date: 2019-03-28


A sensitive, robust, and selective analytical method for instantaneous determination of  chloramphenicol, tetracyclines and sulfonamides in food of animal origin by cutting-edge LC-MS/MS QTRAP has been established and validated. Sample treatment was based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) with several adjustments depending on the matrix and drugs group.  Double extractions using acetified  acetonitrile with 1% acetic acid are common practice in sample preparation of sulfonamides (SAs) and chloramphenicol (CAP) while extraction for tetracyclines (TCs) was by 98% methanol/2% hydrochloric acid. Extracts were cleaned-up using PSA for the dispersive solid phase extraction step for interference removal. Various conditions such as MS compatible solutions, LC column, mobile phase and gradient elution were tested in order to save analysis time and for efficient chromatographic separation. Optimization of the various MS/MS experimental parameters  (declustering potential, collision cell exit potential, desolvation temperature, gas flow and collision energy) was also carried out by full scan and selective reaction monitoring (SRM) with direct injection of single and mixed standard solutions. Matrix interferences were monitored in extracts of honey and chicken muscles for 12 antibiotics using recently developed and validated methods with Ultra-High LC-MS/MS QTRAP. Although a significant dispersion in the results were observed for most of the compounds, ion suppression was the major issue. The optimized method was validated, obtaining suitable results for all validation parameters in the evaluated matrices. Recovery values ranged from 70% to 120% and repeatability and reproducibility were obtained at values lower than 20%. The limit of quantification (LOQ) was established at 0.20, 10 and 15 µg/kg for CAP, SAs and TCs, respectively, which were lower than the maximum limit legally established by the European Union (EU). Reference materials (CRMs) and proficiency tests (PTs) samples were simultaneously performed to improve confidence in the measurement results. A full in-house validation of the method intended for routine analysis to support regulatory enforcement.  Finally, the method was applied to 150 samples from different matrices (honey, chicken, liver etc.).


Chloramphenicol, tetracyclines, sulfonamides, food of animal origin, method optimization

Journal: Journal of Food, Agriculture and Environment
Year: 2019
Volume: 17
Issue: 2
Category: Food and Health
Pages: 12-20

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