Development and validation of a method for the determination of low-ppb levels of macrocyclic lactones in butter, using HPLC-fluorescence

Food Chem. 2015 Jul 15:179:239-45. doi: 10.1016/j.foodchem.2015.01.046. Epub 2015 Feb 7.

Abstract

An analytical method was developed and validated for the simultaneous determination of four macrocyclic lactones (ML) (abamectin, doramectin, ivermectin and moxidectin) in butter, using liquid chromatography with fluorescence detection. The method employed heated liquid-liquid extraction and a mixture of acetonitrile, ethyl acetate and water, with preconcentration and derivatization, to produce stable fluorescent derivatives. The chromatographic run time was <12.5 min, with excellent separation. The method validation followed international guidelines and employed fortified butter samples. The figures of merit obtained, e.g. recovery (72.4-106.5%), repeatability (8.8%), within-laboratory reproducibility (15.7%) and limits of quantification (0.09-0.16 μg kg(-1)) were satisfactory for the desired application. The application of the method to real samples showed that ML residues were present in six of the ten samples evaluated. The method proved to be simple, easy and appropriate for simultaneous determination of ML residues in butter. To our knowledge, this is the first method described for the evaluation of ML in butter.

Keywords: Avermectins; Butter analysis; Dairy product; HPLC-fluorescence; Method validation; Veterinary drug residues.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Butter / analysis*
  • Calibration
  • Chromatography, High Pressure Liquid / methods*
  • Lactones / analysis*
  • Reproducibility of Results
  • Spectrometry, Fluorescence

Substances

  • Lactones
  • Butter