Analysis of Veterinary Drug and Pesticide Residues Using the Ethyl Acetate MulticlassMultiresidue Method in Milk by Liquid Chromatography-Tandem Mass Spectrometry

Abstract EN

A rapid and simple multiclass, ethyl acetate (EtOAc) multiresidue method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) detection was developed for the determination and quantification of 26 veterinary drugs and 187 total pesticide residues in milk.

Sample preparation was a simple procedure based on liquid–liquid extraction with ethyl acetate containing 0.1% acetic acid, followed by centrifugation and evaporation of the supernatant.

The residue was dissolved in ethyl acetate with 0.1% acetic acid and centrifuged prior to LC-MS/MS analysis.

Chromatographic separation of analytes was performed on an Inertsil X-Terra C18 column with acetic acid in methanol and water gradient.

The repeatability and reproducibility were in the range of 2 to 13% and 6 to 16%, respectively.

The average recoveries ranged from 75 to 120% with the RSD ( n = 18 ).

The developed method was validated according to the criteria set in Commission Decision 2002/657/EC and SANTE/11945/2015.

The validated methodology represents a fast and cheap alternative for the simultaneous analysis of veterinary drug and pesticide residues which can be easily extended to other compounds and matrices.